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Eingeladener Vortrag
- nein (66)
Volatile organic compounds (VOCs) emitted by furniture and building materials can cause health issues. For an improvement of indoor air quality low emitting materials should be used. Quality assurance and –control (QA/QC) measures require an emission reference material (ERM) with a predictable emission rate of VOCs. The idea is to use porous materials as ERM, which store the VOCs inside their pores and emit them constantly.
The emission of ultrafine particles from small desktop Fused Filament Fabrication (FFF) 3D printers has been frequently investigated in the past years. However, the vast majority of FFF emission and exposure studies have not considered the possible occurrence of particles below the typical detection limit of Condensation Particle Counters and could have systematically underestimated the total particle emission as well as the related exposure risks. Therefore, we comparatively measured particle number concentrations and size distributions of sub-4 nm particles with two commercially available diethylene glycol-based instruments – the TSI 3757 Nano Enhancer and the Airmodus A10 Particle Size Magnifier. Both instruments were evaluated for their suitability of measuring FFF-3D printing emissions in the sub-4 nm size range while operated as a particle counter or as a particle size spectrometer. For particle counting, both instruments match best when the Airmodus system was adjusted to a cut-off of 1.5 nm. For size spectroscopy, both instruments show limitations due to either the fast dynamics or rather low levels of particle emissions from FFF-3D printing in this range. The effects are discussed in detail in this article. The findings could be used to implement sub-4 nm particle measurement in future emission or exposure studies, but also for the development of standard test protocols for FFF-3D printing emissions.
In industrialised countries more than 80% of the time is spent indoors. Products, such as building materials and furniture, emit volatile organic compounds (VOCs), which are therefore ubiquitous in indoor air. VOC in combination may, under certain environmental and occupational conditions, result in reported sensory irritation and health complaints. Emission concentrations can become further elevated in new or refurbished buildings where the rate of air exchange with fresh ambient air may be limited due to improved energy saving aspects. A healthy indoor environment can be achieved by controlling the sources and by eliminating or limiting the release of harmful substances into the air. One way is to use (building) materials proved to be low emitting. Meanwhile, a worldwide network of professional commercial and non-commercial laboratories performing emission tests for the evaluation of products for interior use has been established. Therefore, comparability of test results must be ensured. A laboratory’s proficiency can be proven by internal and external validation measures that both include the application of suitable emission reference materials (ERM). For the emission test chamber procedure according to EN 16516, no artificial ERM is commercially available. The EU-funded EMPIR project MetrIAQ aims to fill this gap by developing new and improved ERMs. The goal is to obtain a material with a reproducible and temporally constant compound release (less than 10 % variability over 14 days). Two approaches were tested: the impregnation of porous materials with VOC, and the encapsulation of VOC in polymer microcapsules. Impregnation is performed with help of an autoclave and supercritical CO2. The encapsulation is done by interfacial polymerisation on VOC droplets. For both approaches, synthesis and/or material parameters were varied to obtain an optimal ERM. Findings about the optimisation of ERM generation, as well as performance of the best emission reference materials, will be presented.
Nowadays, people spend most of their time indoors. Thus, a good indoor air quality is important. Emissions of volatile organic compounds (VOCs) from furniture and building materials can cause health complaints1. Quantitative VOC-emission testing is carried out under standardized conditions in emission test chambers. In the presented project an emission reference material (ERM) is developed that emits a defined mixture of VOCs which is required for quality assurance and -control (QA/QC) measures. Porous materials (e.g zeolites, activated carbons, MOFs or aerogels) are used as reservoir materials and impregnated with VOC. The porous materials are selected, among others, by their pore size, pore size distribution, polarity and availability. Due to their regular pore structure zeolites are tested at first. For a prediction of the emission profile, the ERM is supposed to exhibit a constant emission rate over time. The aim is a stability of ≤ 10 % change in the emission rate over a minimum of 14 days.
Method
For impregnation, the material is placed into an autoclave inside a rotatable basket. The VOC is added and the autoclave is closed. Afterwards, CO2 is inserted. The closed system is then heated to the supercritical point of CO2 (31 °C, 73.75 bar). In this state, the CO2 acts as solvent for the VOC. By rotating the basket, the distribution of the VOC is ensured. After a few minutes, the pressure is decreased slowly and the CO2 is released. For the determination of the emission profile, the impregnated sample is placed into an emission test chamber. These chambers can be operated either with dry or humid air (50 ± 5 % rel. humidity). Every second to third day, air samples are taken and analyzed by gas chromatography. For an ideal impregnation, several different pressures and temperatures as well as impregnation times are tested.
Results
Two zeolite materials tested in dry air conditions reach emission profiles with a decrease of less than 10 % over 14 days (heptane and toluene, respectively). Further it was discovered that smaller pellets of the same zeolite show better results than bigger particles. When the pore size of a zeolite is too small, e.g. 0.3 nm, the VOC cannot be absorbed sufficiently. The main disadvantage of zeolites is their hygroscopicity because it has a large impact on the release of VOC when they are used in emission test chambers under standardized test conditions (23 °C, 50 % rel. humidity). Activated carbons have emission profiles with a larger change over 14 days. However, the high hydrophobicity allows measurements in humid air conditions which was not possible with the before mentioned hygroscopic zeolites. It is possible to impregnate powdered materials as well, and thus powdered non-hygroscopic (n.h.) zeolites were impregnated. Their emission profiles are comparable to those of the activated carbons. The use of methylated hygroscopic zeolites with a decrease in hygroscopicity did not yield successful emission measurements. The change over 14 days is calculated only for the stable phase (~250–300 h).
The desired stability of ≤ 10 % change of the emission rate over 14 days could already be reached under dry testing conditions. Further investigations under humid conditions show that zeolites with high Si/Al-ratios are non-hygroscopic and comparable to activated carbons (20–30 % change). The next step is to reduce the change in the emission rate of these materials to the aimed ≤ 10 % over 14 days.
Microbiologically influenced corrosion (MIC) is a crucial issue for industry and infrastructure. Biofilms are known to form on different kinds of surfaces such as metal, concrete, and medical equipment. However, in some cases the effect of microorganisms on the material can be negative for the consistency and integrity of the material. Thus, to overcome the issues raised by MIC on a system, different physical, chemical, and biological strategies have been considered; all having their own advantages, limitations, and sometimes even unwanted disadvantages. Among all the methods, biocide treatments and antifouling coatings are more common for controlling MIC, though they face some challenges. They lack specificity for MIC microorganisms, leading to cross-resistance and requiring higher concentrations. Moreover, they pose environmental risks and harm non-target organisms. Hence, the demand for eco-friendly, long-term solutions is increasing as regulations tighten. Recently, attentions have been directed to the application of nanomaterials to mitigate or control MIC due to their significant antimicrobial efficiency and their potential for lower environmental risk compared to the conventional biocides or coatings. Use of nanomaterials to inhibit MIC is very new and there is a lack of literature review on this topic. To address this issue, we present a review of the nanomaterials examined as a biocide or in a form of a coating on a surface to mitigate MIC. This review will help consolidate the existing knowledge and research on the use of nanomaterials for MIC mitigation. It will further contribute to a better understanding of the potential applications and challenges associated with using nanomaterials for MIC prevention and control.
In 2005, a team of Polish archaeologists discovered three Coptic codices, two on papyrus and one on parchment, in the rubbish dump of a hermitage at Sheik Abd el-Gurna, Egypt. While the parchment codex and the remains of the bindings of the papyrus ones have been conserved, the text blocks of the papyrus codices were opened and disassembled and after being disinfected remained untouched for nearly 15 years, until the current project started. Currently, all three books are stored in the collection of the Coptic Museum in Cairo. Our team undertook the conservation of and archaeometric research on the papyrus codices. The first of the books contains the Canons of Pseudo-Basil, while the second is an Encomium of St. Pisenthios. Both codices have been palaeographically dated to the seventh-eighth centuries CE. In this paper, we describe our project and present the results of the work carried out on the Canons of Pseudo-Basil. Our work involved photography in transmitted light, measurements of the thickness of the papyrus leaves, and digital microscopy under three-light illumination. These measurements allowed us to determine the types of the inks and characterize the papyrus writing substrate. For conservation, we used a novel method developed in the Egyptian Museum in Berlin that comprises suspending papyrus folios on a translucent, extremely thin Japanese paper inside glass frames without the use of adhesives.In 2005, a team of Polish archaeologists discovered three Coptic codices, two on papyrus and one on parchment, in the rubbish dump of a hermitage at Sheik Abd el-Gurna, Egypt. While the parchment codex and the remains of the bindings of the papyrus ones have been conserved, the text blocks of the papyrus codices were opened and disassembled and after being disinfected remained untouched for nearly 15 years, until the current project started. Currently, all three books are stored in the collection of the Coptic Museum in Cairo. Our team undertook the conservation of and archaeometric research on the papyrus codices. The first of the books contains the Canons of Pseudo-Basil, while the second is an Encomium of St. Pisenthios. Both codices have been palaeographically dated to the seventh-eighth centuries CE. In this paper, we describe our project and present the results of the work carried out on the Canons of Pseudo-Basil. Our work involved photography in transmitted light, measurements of the thickness of the papyrus leaves, and digital microscopy under three-light illumination. These measurements allowed us to determine the types of the inks and characterize the papyrus writing substrate. For conservation, we used a novel method developed in the Egyptian Museum in Berlin that comprises suspending papyrus folios on a translucent, extremely thin Japanese paper inside glass frames without the use of adhesives.
Die Bezeichnung „Tinte auf Papier“ bietet einen guten Einstieg in die Beschreibung der Materialität von Musikhandschriften; so haben sich zahlreiche Manuskripte erhalten, die mit Eisengallustinte auf Hadernpapier verfasst wurden.
Das Papier besteht aus Fasern meist pflanzlicher Herkunft und wird durch Entwässerung einer Fasersuspension auf einem Sieb gebildet. Der Abdruck des Schöpfsiebes (die Papierstruktur) und ein vorhandenes Wasserzeichen bieten Anhaltspunkte für Provenienz und Datierung; daneben erlaubt die Analyse der Fasern, der Füllstoffe und der Leimung eine weitere Charakterisierung des Schriftträgers.
Spätestens seit dem Mittelalter sind es Eisengallustinten, die das schwarze bis bräunliche Erscheinungsbild vieler Manuskripte auf Papier hervorrufen. Daneben lassen sich auch schwarze Rußtuschen oder farbige Auszeichnungstuschen nachweisen. Eisengallustinten werden durch Mischung einer eisenhaltigen Komponente mit Gerbstoffen hergestellt. Eisensulfat ist die am häufigsten genannte Eisen liefernde Zutat, daneben sind aber auch eisenhaltige Minerale, Nägel oder Rost denkbar. Die Gallussäure leitet sich ab aus den Galläpfeln, der krankhaften Veränderung einzelner Planzenteile verschiedener Eichenarten. Diese werden durch die Eiablage von Schlupfwespen hervorgerufen.
Wie schon beim Papier ermöglicht der materialanalytische Nachweis charakteristischer Beimischungen oder Verunreinigungen innerhalb der Tinten die Beantwortung kulturhistorischer Fragestellungen – gemeint sind hier die Unterscheidung von Original und Korrektur oder die Sichtbarmachung späterer Ergänzungen.
Black writing materials of different types and compositions have varied in use over time and different geographical regions. With this paper, we would like to contribute to their study by listing and reviewing recipes for black writing inks that were in circulation in the Carolingian Empire as well as by referencing the archaeometric analyses of the black inks used in the manuscripts. The studies presented here that involved the humanities and natural sciences provide new insights into how the scholars of the early Medieval Ages organized manuscripts.
Colours on East Asian Maps
(2023)
Maps and colours have a close connection. Drawn or printed in black on white, subsequently added colours enhance maps with additional information. Colours were not just there to improve maps aesthetically, but they regulated how they were read and thus reinforced their meanings, significances and ideas. Colour is an important key to a more precise understanding of the map’s purposes and uses; moreover, colours are also an important aspect of a map’s materiality. The material scientific analysis makes it possible to find out more about the making of colours and the process of colouring maps. By skillfully deploying colours, map colourists were able to create mimetic representations of nature or codify information in an abstract form. The use of colours involved many considerations as to the materials. ‘Reading’ colours in this way gives a glimpse into the social lives of mapmakers as well as map users and reveals the complexity of the historical and social context in which maps were produced and how the maps were actually made. Within the scope of the three-year joint research project Coloured Maps (2018–2021), we undertook an in-depth and systematic study of hand-drawn and hand-coloured maps from East Asia in the Museum am Rothenbaum (MARKK) in Hamburg and produced between the seventeenth and twentieth centuries.
With a multi-perspective approach and transdisciplinary methods (humanities and the sciences), we were able to pool and compare the research results from different fields of research on Asian maps. The aim of this publication is to provide a first general overview of the subject of colours on maps in East Asia in the period from the seventeenth to the early twentieth century and to stimulate further research on the topic.
Der Vortrag widmet sich der materialwissenschaftlichen Analyse von Zeichnungen einiger Bauhausschülerinnen und Bauhausschüler und legt besonderen Fokus auf die verwendeten Farbmittel. Die Objekte werden mit nicht-invasiven bildgebenden Verfahren untersucht, in dem die Wechselwirkung zwischen Röntgen-, sichtbarem und infraroten Licht und den Zeichnungen studiert wird.
Dier Analysen liefern nicht nur generell Erkenntnisse über die Art und Zusammensetzung und damit das Alter der verwendeten Farbmittel. Durch die Auffindung von Vorzeichnungen, die Bestimmung von Überarbeitungen und Korrekturen werden Erkenntnisse über die Genese von Zeichnungen gewonnen. Auf der Basis dieser materialwissenschaftlichen Erkenntnisse werden die Begriffe Original, Kopie, Fälschung diskutiert.
Da die nicht-invasiven Untersuchungen einen umfassenden Einblick in die Materialität der – überwiegend aus Papier bestehenden – Objekte erlauben, bilden sie die Grundlage für die Erstellung nachhaltiger Konservierungs- und Restaurierungskampagnen und deren dauerhaften Erhalt.
In this article, we present two Coptic papyri, P 11934 and P 11935 from the Berlin collection excavated in Ashmunein (ancient Hermopolis) by Otto Rubensohn in 1906. We employ a multi-disciplinary approach that takes into account both their materiality – writing support as well as ink – and their content, as has become ‘best practice’. 1 Material aspects of written documents have traditionally been the purview of papyrologists. Recently developed methods of scientific analysis generate sets of archaeometric data with the potential to improve understanding of the materiality of ancient document production, as well as to yield new evidence for genuine papyrological research questions. To achieve this, a large corpus of comparative data needs to be built. Our contribution offers a first step in this direction. We aim at presenting the papyri, which were selected because of the ink corrosion during conservation work at the Berlin collection, in a format that is exhaustive both for material and textual aspects. The inks from both papyri were analysed using a combination of techniques, contributing to our better understanding of the development of ink technology in Late Antiquity.
Volatile organic compounds (VOCs) emitted by furniture and
building materials can cause health issues. For an
improvement of indoor air quality low emitting materials
should be used. Quality assurance and –control (QA/QC)
measures require an emission reference material (ERM) with a
predictable emission rate of VOCs. The idea is to use porous
materials as ERM, which store the VOCs inside their pores and
emit them constantly.
Conclusion et piste:
Il semblerait qu’il n’existe pas de corrélation entre le type d’encre utilisés et d’autres critères recherchés à part une marque de préférence personnelle, sauf en ce qui concerne des documents religieux, auquel cas une différence se fait en function de la communauté.
Les résultats réunis dans cette étude semble indiquer que les scribes achètent leur propre encre.
L’analyse des encres peut nous aider à retracer une chronologie de l’écriture et signature de certains documents juridiques.
Élargissement du corpus:
- Comparaison avec des documents écrits par la cour du Qadi
- Documents d’autres collections
- Avec d’autres documents contemporains (Génizah Afghane)
In recent years the BAM has been focusing on the characterization of the writing materials of the medieval Torah scrolls. The challenge imposed by the study of this specific type of manuscript led to designing and building dedicated stages to ensure the safety of the scrolls during the analysis. Furthermore, the identification of multiple corrections executed in apparently identical inks required broadening the standard two-step protocol of near infrared reflectography and X-ray fluorescence to include multispectral imaging. This work has prepared the division to participate in the large collaborative project “To roll: Materialisierte Heiligkeit (Materialised Holiness)” based at the Free University, Berlin.
The presentation will demonstrate the aims of the studies, preliminary results and the strategies adopted by the division 4.5 of the BAM.
The ink analysis protocol developed through cooperation between the Bundesanstalt für Materialforschung und -prüfung in Berlin and the Centre for the Study of Manuscript Cultures at the University of Hamburg involves the use of imaging techniques for ink screening, followed by spectroscopic analysis. In our presentation, we will begin by briefly reviewing the history of writing inks and discussing the three main categories: carbon-based inks, plant, and iron-gall inks. We will address their chronology, precursors, and mixed forms, as well as the features that allow for their identification. Then, we will present the techniques we use in ink analysis, whereby we would like to highlight the limitations, advantages, and disadvantages of each approach. Finally, we will discuss the new mass-spectrometric method based on micro-sampling and using atmospheric solid analysis probe (ASAP).
The current state of preservation of the DSS results from the synergetic effect of various factors such as great age, post-discovery treatments, poor storage conditions, environmental influences and exhibitions. With rare exceptions, neither the initial state nor a list of the treatments performed on each DSS fragment is known. Reconstruction of the individual fragment history will have to rely upon advanced analytical techniques to identify the treatments and their effects.
Management of the scrolls may be divided roughly into three periods: a) the scholarly archiving period, from 1948 to the mid-1960s; b) first attempts at conservation, from the mid-1960s to late-1980s; c) Israel Antiquities Authority Scrolls Lab, from 1991 onwards.
Physico-chemical analyses of writing materials offer insight into various questions associated with historical, cultural, and conservational aspects of manuscript studies. The catalogue of questions that can be addressed with these methods includes authenticity, dating, the attribution of various parts of the text to different scribes and the relation between the primary and secondary texts. Similarly, preservation of the manuscripts requires knowledge of the composition of the original materials versus old repairs, identification of damage, as well as recognition of natural aging and degradation processes. The material sciences can contribute data about the chemical compositions of the writing materials, elucidation of the techniques of their production and the absolute age of organic components, as well as characterization of corrosion effects, evaluation of conservation treatment, and monitoring of the preservation state.
Ancient Inks
(2023)
In the last decade scientists and scholars have accumulated more knowledge on black ink used for writing in Antiquity and the early Middle Ages.
Ready availability of non-destructive testing instruments employed in interdisciplinary projects on historic manuscripts have made it possible to determine the composition of ink and to compare it with the extant records.
Interest in the type of skin used in scriptural materials and preparation methods increased from the nineteenth into the twentieth century. This was due partly to the number of newly discovered fragments and to the invention of new instruments and scientific procedures to identify animal skins and produce qualitative means to demonstrate specific preparation reagents and techniques. The invention of various means of analyzing the DNA of organic materials brought about a revolution in archaeology and in conservation. Difficulties in overcoming contamination of archaeological samples resulted in a number of controversies but also produced advances and improvement in the techniques of ancient DNA analysis and interpretation of results.
On the use of Carbograph 5TD as an adsorbent for sampling VVOCs: validation of an analytical method
(2023)
A standardised method for the analysis of very volatile organic compounds (VVOCs) in indoor air is still missing. This study evaluates the use of Carbograph 5TD as an adsorbent for 60 compounds (47 VVOCs + 13 VOCs) by comparing their recoveries with different spiking modes. The influence of the spiking of the tubes in dry nitrogen, humidified air or along the whole flushing duration mimicking real sampling was investigated. 49 substances (36 VVOCs from C1 to C6) had recoveries over 70% on the adsorbent in humidified air and were validated. The linearity of the calibration curves was verified for every spiking mode and the limits of detection (LOD) and quantification (LOQ) were determined. The LOQs were lower than the existing indoor air guideline values. The robustness of the method was considered by studying the influence of the sampling volume, the sampling flow rate, the humidity level and the storage of the tubes. In general, the most volatile or polar substances were the less robust ones. The combined measurement uncertainty was calculated and lies below 35% for a vast majority of the substances. An example of an emission chamber test using polyurethane foam is shown: Carbograph 5TD performs much better than Tenax® TA for VVOCs and emissions from n-butane were quantified with combined measurement uncertainty.
EN 16516 sets specifications for the determination of emissions into indoor air from construction products. Reliable, accurate and International System of Unit (SI)-traceable measurement results of the emissions are the key to consumer protection. Such measurement results can be obtained by using metrologically traceable reference materials. Gas-phase standards of volatile organic compounds (VOCs) in air can be prepared by a variety of dynamic methods according to the ISO 6145 series. However, these methods are not always applicable for semi-VOCs (SVOCs) due to their high boiling point and low vapour pressure. Therefore, a novel dynamic gas mixture generation system has been developed. With this system gas-phase standards with trace level VOCs and SVOCs in air can be prepared between 10 nmol mol−1 and 1000 nmol mol−1. The VOCs and SVOCs in this study have normal boiling points ranging from 146 °C to 343 °C. Metrologically traceable reference materials of the gas-phase standard were obtained by sampling of the VOC gas-phase standard into Tenax TA® sorbent material in SilcoNert® coated stainless steel tubes. Accurately known masses between 10 ng and 1000 ng per VOC were sampled. These reference materials were used to validate the dynamic system. Furthermore, the storage and stability periods of the VOCs in the reference materials were determined as these are crucial characteristics to obtain accurate and SI-traceable reference materials. In a round robin test (RRT), the reference materials were used with the aim of demonstrating the feasibility of providing SI-traceable standard reference values for SVOCs for interlaboratory comparison purposes. Based on the results from the validation, the storage and stability studies and the RRT, gas-phase standards and reference materials of VOCs and SVOCs with relative expanded uncertainties between 5% and 12% (k = 2) have been developed. These reference standards can be used as calibrants, reference materials or quality control materials for the analysis of VOC emissions.
VOC-emissions and their odours from building products and furnishings present indoors should not have an impact on personal well-being or health. Odours can be measured by applying the standard ISO 16000-28. Indoor air determination of odour emissions from building products using test chambers. One of the described procedures is the assessment of perceived intensity using a comparative scale by a group of panellists. In this paper, the perceived intensity sampling procedure and its evaluation method are investigated and shown to need improvement. New technical developments in the methodology used to increase the reproducibility of measurement results are discussed. Since odour tests are used for labelling, they have a major influence on the assessment of construction products, similar to the procedure of the German Committee for Health Evaluation of Building Products (AgBB). In the original ISO standard, the evaluation is typically performed using a sampling container separated from the emission chamber. For a better sample presentation, an adapter was developed to connect the emission test chamber to the evaluation funnel and thus enable an odour assessment which is comparable to a direct measurement. The investigations show that losses of odourous substances can be greatly reduced, which is very desirable when seeking to obtain reliable results in odour measurement. Another experimental series was carried out to reduce the measurement effort in the evaluation of perceived intensity. Application of the developed greater than or less than/equal to. query could be helpful here. The results show that the query mostly leads to the same result as the evaluation of the perceived intensity using the method according to the standard but is much easier to perform. Overall, the results can contribute to improving the acceptance of the evaluation of perceived intensity using ISO 16000-28 and to determining odours from building materials increasingly more precisely.
Fused filament fabrication (FFF) on desktop 3D printers is a material extrusion-based technique often used by educational institutions, small enterprises and private households. Polymeric filaments are melted and extruded through a heated nozzle to form a 3D object in layers. The extrusion temperature is therefore a key parameter for a successful print job, but also one of the main driving factors for the emission of harmful air pollutants, namely ultrafine particles and volatile organic gases, which are formed by thermal stress on the polymeric feedstock. The awareness of potential health risks has increased the number of emission studies in the past years. However, the multiplicity of study designs makes an objective comparison of emission data challenging because printer hardware factors such as the actual extruder temperature (TE) and also feedstockspecific emissions are not considered. We assume that across the market of commercial low- and mid-price FFF printers substantial deviations between actual and set extruder temperatures exist, which have a strong effect on the emissions and hence may bias the findings of exposure studies. In our last publication, we presented a standardized feedstock-specific emission test method and showed that for each investigated feedstock an increase in actual extruder temperature was accompanied by an increase in particle emissions (Tang and Seeger, 2022). Therefore, any systematic discrepancy between set and actual extruder temperature matters. In this study, we used a thermocouple and an infrared camera to measure the actual extruder temperatures at different heights. We found significant under- and overestimation of the actual extruder temperatures by the respective set temperatures in three commercial printers. This caused a broad variation of the measured total numbers of emitted particles (TP), even when the same feedstock was operated. For the determination of TP, we followed the DE-UZ 219 test guideline. In a second round we repeated the tests with all printers adjusted to exactly the same extruder temperatures, i.e., to TE=230°C for ABS and TE=210°C for PLA. All measurements were conducted in a 1 m³ emission test chamber. Particle emissions in the size range between 4 nm and 20 μm were detected. Printing on three different printer models without temperature adjustment resulted for each of the investigated feedstocks in a variation in TP of around two orders of magnitude. After temperature adjustment, this was substantially reduced to approx. one order of magnitude and hence minimizes the bias of printer hardware on the emissions. Our findings suggest that adjustment of the extruder temperature should be mandatory in emission testing standards. It also poses a more accurate benchmark and provides more reliable emission data for evaluation of indoor air quality or for health risk assessments. In addition, a proper temperature setting is in the interest of the user. Some commercial FFF printers may have a higher actual extruder temperature than displayed and unintended overheating may not only impair the print quality but may cause unnecessarily increased exposure to particle emissions.
Fused filament fabrication (FFF) is a material extrusion-based technique often used in desktop 3D printers. Polymeric filaments are melted and are extruded through a heated nozzle to form a 3D object in layers. The extruder temperature is therefore a key parameter for a successful print job but also one of the main emission driving factors as harmful pollutants (e.g., ultrafine particles) are formed by thermal polymer degradation. The awareness of potential health risks has increased the number of emission studies in the past years. However, studies usually refer their calculated emission data to the printer set extruder temperature for comparison purposes. In this study, we used a thermocouple and an infrared camera to measure the actual extruder temperature and found significant temperature deviations to the displayed set temperature among printer models. Our result shows that printing the same filament feedstocks with three different printer models and with identical printer set temperature resulted in a variation in particle emission of around two orders of magnitude. A temperature adjustment has reduced the variation to approx. one order of magnitude. Thus, it is necessary to refer the measured emission data to the actual extruder temperature as it poses a more accurate comparison parameter for evaluation of the indoor air quality in user scenarios or for health risk assessments.
Emission testing of volatile organic compounds (VOC) from materials and products is commonly based on emission test chamber measurements. To ensure the comparability of results from different testing laboratories their measurement performance must be verified. For this purpose, Bundesanstalt für Materialforschung und -prüfung (BAM) organizes an international proficiency test every two years using well-characterised test materials (one sealant, one furniture board and four times a lacquer) with defined VOC emissions. The materials fulfilled the requirements of homogeneity, reproducibility, and stability. Altogether, 41 VOCs were included of which 37 gave test chamber air concentrations between 10 and 98 µg/m³. This is the typical concentration range to be expected and to be quantified when performing chamber tests. Four compounds had higher concentrations between 250 and 1105 µg/m³. The relative standard deviations (RSD) of BAM proficiency tests since 2008 are compared and the improvement of the comparability of the emission chamber testing is shown by the decrease of the mean RSD down to 23% in 2021. In contrast, the first large European interlaboratory comparison in 1999 showed a mean RSD of 51%.
In industrialised countries more than 80% of the time is spent indoors. Products, such as building materials and furniture, emit volatile organic compounds (VOCs), which are therefore ubiquitous in indoor air. Different VOC combinations may, under certain environmental and occupational conditions, result in reported sensory irritation and health complaints. A healthy indoor environment can be achieved by controlling the sources and by eliminating or limiting the release of harmful substances into the air. One way is to use materials proven to be low emitting. Meanwhile, a worldwide network of professional commercial and non-commercial laboratories performing emission tests for the evaluation of products for interior use has been established. Therefore, comparability and metrological traceability of test results must be ensured. A laboratory’s proficiency can be proven by internal and external validation measures that both include the application of suitable reference materials. The emission test chamber procedure according to EN 16516 comprises several steps from sample preparation to sampling of test chamber air and chromatographic analysis. Quality assurance and quality control (QA/QC) must therefore be ensured. Currently, there is a lack of suitable reference products containing components relevant for the health-related evaluation of building products.
The EU-funded EMPIR project 20NRM04 MetrIAQ (Metrology for the determination of emissions of dangerous substances from building materials into indoor air) aims to develop 1) gaseous primary reference materials (gPRM), which are used for the certification of gaseous (certified) reference materials (gCRM) and 2) emission reference materials (ERM).
Most commercial gas standards of indoor-relevant compounds are not certified due to the lack of primary reference materials to which the project aims to contribute. The gPRM under development is a gas-phase standard containing trace levels of VOCs in nitrogen or air from the check standard according to EN 16516 (n-hexane, methyl isobutyl ketone, toluene, butyl acetate, cyclohexanone, o-xylene, phenol, 1,3,5-trimethylbenzene) with a target uncertainty of 5 %. The gPRM can be sampled into sorbent tubes to obtain transfer standards in the form of gCRM.
The well characterised ERM represents a sample of a test specimen, e.g. building material, that is loaded into the emission test chamber for a period of several days and is used to evaluate the whole emission test chamber procedure. It shall have a reproducible and temporally constant compound release of less than 10 % variability over 14 days. Different approaches for retarded VOC release, such as the encapsulation of pure compounds and the impregnation of porous materials, are being tested to reach this aim. Furthermore, the design of the ERM is accompanied by the development of a numerical model for the prediction of the emissions for each of the target VOCs. The current progress of the work on both materials will be presented.
Round robin tests of odour and VOC emissions from building products – What have we learned so far?
(2023)
Emission testing of volatile organic compounds (VOC) and odour from materials and products is commonly based on emission test chamber measurements. These measurements are often the basis of mandatory or voluntary labelling procedures. To ensure the comparability of results from different testing laboratories their performance must be verified. For this purpose, round robin tests (RRTs) are conducted. Bundesanstalt für Materialforschung und - prüfung (BAM) offers such a RRT every two years using well characterised test materials with defined VOC emissions. In addition to the VOC quantification, the evaluation of odour is also implemented in the round robin tests. At the beginning, only perceived intensity (PI) was tested but over the years also the acceptance evaluation was considered. In principle, the results of PI and acceptance evaluation are comparable. The advantage of PI is the lower number of panel members necessary for one evaluation.
In an interdisciplinary collaboration, restorers, art historians, and scientists examined Guilio Romano’s The Madonna with the Wash-Basin of 1525 (Dresden State Art Collections). Insights into the painting technique along with art historical comparisons provided the opportunity for a better understanding of the painting’s genesis, in particular concerning an early reworking of the background by the artist. A recovery and reconstruction of the earlier version of the background is now possible. The discovery of zinc in distinct passages of the painting, as well as the grey-black pigment stibnite and glass particles used as a supplement in paint layers are of special interest. The technological investigation initiated a discussion about the circumstances of the revision, as well as the painting’s relation to Vasari’s Lives of Artists.
Hundreds of papyrus rolls, carbonized during the 79CE eruption of Mount Vesuvius, were discovered in 1754 at Herculaneum. Sophisticated mechanical methods for unrolling the best-preserved scrolls have been applied, with varying success. However, such processes have been abandoned, to prevent risk from irremediable damage or loss and to preserve the integrity of the extremely fragile rolls. Following the development of X-ray based non-invasive techniques, attempts to virtually unroll the scrolls were made. The most common ink in Antiquity was carbon-based, and the main element of carbonized papyrus is carbon, making these investigations difficult. However, some attempts with synchrotron X-ray phase-contrast tomography (XPCT) were successful. Recently, the identification of antique inks containing metals raised hope that if some of the inks contain metal the rolls can be virtually unrolled using conventional CT- technique. We investigated the inks of a selection of partially unrolled fragments stored at the Biblioteca Nazionale di Napoli with X-ray fluorescence in order to select the best candidates for tomography. Despite the many difficulties (analysis of several layers sticking together, letters barely visible, difficulty to separate contribution from the ink and from the papyrus, inhomogeneity of the support, fragility of the fragments…), encouraging results were found, with a number of inks from Greek fragments found to contain additions to the soot (Fe, Pb, Cu P).
Generation of experimental uptake rates (UR) for > 70 VOCs (7d /100 μg m-3)
Application in German Environmental Survey – VOC exposure assessment
Assurance of transparency concerning UR generation and uncertainty creates basis for decision making and comparability of measurement results.
Exemplarily the uncertainty u(UR) of toluene UR was modelled and determined statistically with own laboratory data (relative standard deviation of actively sampled test gas atmosphere – RSDa and n = 5 exposed passive samplers – RSDp) in line with EN 838 as well as from variation of literature UR – RSD UR,lit.
Die Klassik-Stiftung Weimar besitzt eine umfangreiche Sammlung niederländischer und flämischer Zeichnungen vom 15. bis 19. Jahrhundert. Im Rahmen des Forschungsprojektes »Kennerschaft heute« wurde der Bestand der über 1.500 Zeichnungen erstmals wissenschaftlich erschlossen. Das Handbuch führt anhand bedeutender Werkgruppen, darunter Zeichnungen von Lucas van Leyden, Dirck Vellert, Roelant Savery und Rembrandt, den Reichtum der Weimarer Sammlung vor Augen, die zum großen Teil auf die Sammelleidenschaft von Johann Wolfgang Goethe zurückgeht. Im Zentrum des Buches steht aber die Zusammenarbeit von traditioneller Stilkritik und naturwissenschaftlicher Materialanalyse. In zwölf Fallbeispielen wird die Notwendigkeit einer methodischen Neuausrichtung der Kennerschaft darlegt. Einen Schwerpunkt der Untersuchungen bildet hierbei das große Konvolut an Zeichnungen von Rembrandt und seinen Schülern, das erstmals systematisch auf die verwendeten Zeichenmaterialien und Papiere untersucht wird.
Der fabelhafte Möglichmacher
(2022)
Hundreds of papyrus rolls, carbonized during the 79CE eruption of Mount Vesuvius, were discovered in 1754 at Herculaneum. Sophisticated mechanical methods for unrolling the best-preserved scrolls have been applied, with varying success. However, such processes have been abandoned, to prevent risk from irremediable damage or loss and to preserve the integrity of the extremely fragile rolls. Following the development of X-ray based non-invasive techniques, attempts to virtually unroll the scrolls were made. The most common ink in Antiquity was carbon-based, and the main element of carbonized papyrus is carbon, making these investigations difficult. However, some attempts with synchrotron X-ray phase-contrast tomography (XPCT) were successful. Recently, the identification of antique inks containing metals raised hope that if some of the inks contain metal the rolls can be virtually unrolled using conventional CT- technique. We investigated the inks of a selection of partially unrolled fragments stored at the Biblioteca Nazionale di Napoli with X-ray fluorescence in order to select the best candidates for tomography. Despite the many difficulties (analysis of several layers sticking together, letters barely visible, difficulty to separate contribution from the ink and from the papyrus, inhomogeneity of the support, fragility of the fragments…), encouraging results were found, with a number of inks from Greek fragments found to contain additions to the soot (Fe, Pb, Cu P).
This study will present a new approach to distinguishing writing inks that have the same elemental compositions and visual appearances. The approach is based on displaying the intensity of elemental distributions as heat maps that represent data recorded with a scanning μX-ray fluorescence spectrometer. The heat maps present the data so as to facilitate digitally identifying and distinguishing between inks used to produce, correct, and reink two medieval Torah scrolls. As ritual objects, Torah scrolls had to be written in accordance with exacting standards that evolved over time. This requirement led to successive stages of modifications, sometimes over centuries. Both vitriolic and non-vitriolic inks used to modify Torah scrolls can be visually identical to each other. Furthermore, different non-vitriolic inks usually have an identical elemental composition. The solid material analysis evidence and its presentation as heat maps made it possible to discriminate between original and altered portions of text that in some cases would have been impossible. Our interdisciplinary work brought together conservation, material science, paleog-raphy, and philology to enable the identification of complex stratigraphy in multiple stages of production, correction, and reinking. ©2 0 2 2 Published by Elsevier Masson SAS.
Through the application of scientific methods of analysis to a corpus of medieval manuscripts found in the Cairo Genizah, this work aims to gain a better understanding of the writing materials used by Jewish communities at that time, shedding new light not only on the production of manuscripts in the Middle Ages, but also on the life of those Jewish communities.
Die Publikation befasst sich mit einer einzigartigen Sammlung mexikanischer und südamerikanischer Handschriften, die zu Beginn des 19. Jahrhunderts ins Leben gerufen wurde, als Alexander von Humboldt der Königlichen Bibliothek zu Berlin Fragmente indigener mexikanischer Bilderhandschriften aus dem 16. Jahrhundert schenkte. Sie sind heute auch unter der Bezeichnung Humboldt-Fragmente bekannt und stellen den bedeutendsten Teil der Sammlung dar, die im Laufe der Zeit durch den Ankauf verschiedener Arten von Handschriften aus Mittelamerika, vorwiegend in indigenen Sprachen und lateinischer Schrift, erweitert wurde.
In den zwei Jahren von April 2017 bis März 2019 verfolgten die Staatsbibliothek zu Berlin – Preußischer Kulturbesitz (SBB-PK) und die Bundesanstalt für Materialforschung und -prüfung (BAM) ein gemeinsames, von der Deutschen Forschungsgemeinschaft (DFG) großzügig gefördertes wissenschaftliches Projekt: Materialanalysen und kulturgeschichtliche Untersuchungen mexikanischer Handschriften aus der Kolonialzeit in Berlin und Krakau.
Die Hauptziele des Projekts bestanden darin, die Provenienz der Manuscripta americana zu ermitteln und, da sie einen hohen Grad an Fragmentierung aufweisen, festzustellen, wie sie untereinander und mit Objekten außerhalb der Sammlung in Beziehung stehen. Zu diesem Zweck wurden ethno-kulturhistorische und naturwissenschaftliche Methoden kombiniert. Dank einer guten Zusammenarbeit mit der Jagiellonen-Bibliothek konnten wir die Manuscripta americana sowohl in Berlin als auch in Krakau sehen und studieren und sie wissenschaftlich vermessen.
Der Beitrag beschäftigt sich mit zerstörungsfreien Untersuchungen an den Farbmitteln früher Bauhauszeichnungen. Mit welchen Farbmitteln wurden diese Zeichnungen gestaltet? Wurden hier neueste Zubereitungen genutzt, von denen viele im ersten Drittel des 20. Jahrhunderts gerade auf den Markt kamen, oder fanden – der ebenfalls am Bauhaus propagierten Materialökonomie folgend – althergebrachte Materialien Verwendung, die günstiger zu beschaffen waren? Weitere Fragen widmen sich dem Themenkomplex Original, Kopie und Nachahmung sowie der Auffindung von Fälschungen. Restauratorische, konservatorische und kuratorische Fragestellungen und Entscheidungen sind grundsätzlich damit verknüpft. Zwölf exemplarisch vorgestellte Zeichnungen ermöglichen einen guten Über blick über die verwendeten Farbmittel des frühen Bauhauses von 1919 bis 1925. Trotz der Vielfalt der betrachteten Studien, Entwürfen und Arbeitsblättern, ergibt sich ein homogenes Gesamtbild. Bis auf wenige Ausnahmen dominieren anorganische Pigmente die Farbmittelpalette. Dieser Befund wird durch eine weitaus größere Stichprobe materialtechnologisch untersuchter Zeichnungen aus dem Bestand des Bauhaus-Museums Weimar bestätigt
Results:
- Four types of inks were measured iron gall (vitriolic and non vitriolic), carbonic, mixed and vegetable inks.
- We need to start analyzing systematically the organic part of the inks.
- Great variety in the composition of the inks.
- No correlation between the type of ink used and any other criteria apart from a personal preference.
- Inks purchased by (some) scribes.
- Reconstruction of the chronology of writing and signing of certain legal documents.
- Comparison with documents written by the Muslim court.
Mit der Bezeichnung Hinterglasmalerei wird allgemein der Begriff der Glasmalerei assoziiert. Auch wenn in beiden Fällen Glas das Trägermaterial ist, bezeichnet Hinterglasmalerei jedoch eine völlig andere Technik. Während bei der Glasmalerei die Farben auf den Bildträger eingebrannt werden, handelt es sich bei der Hinterglasmalerei um eine Kaltmalerei. Selbsttrocknende Farben werden auf die Rückseite der Glastafel aufgetragen, zuweilen wird die Malweise durch aufwendige Veredelungstechniken ergänzt. Mehr und mehr rückt diese Technik, die materialtechnologisch zwischen Tafelmalerei und Glasmalerei zu verorten ist, in den Blickwinkel einer interessierten Öffentlichkeit, wie dies eine zunehmende Anzahl verschiedener Ausstellungen zur Hinterglasmalerei belegen. Die vorliegende Publikation beschäftigt sich in erster Linie mit kunsttechnologischen und materialanalytischen Aspekten der Hinterglasmalerei und ermöglicht tiefe Einblicke in die künstlerische Arbeitsweise und in die Verwendung unterschiedlichster Materialien.
The first manuscripts from the Qumran caves were found in 1947. Within the following 10 years, clandestine and legal excavations revealed some 900 highly fragmented manuscripts from the late Second Temple period. This collection is generally known as Scrolls of the Judea Desert or Dead Sea Scrolls (DSS). For many years after their discovery, text analysis and fragmeents attribution were the main concern of the scholars dealing with the scrolls. The uncertain archaeological provenance of the larger part of the collection added an additional difficulty to the formidable task of sorting some 19000 fragments. After 60 years of scholar research the question of origin, archaeological provenance and correct attribution of the fragmenst are still hotly debated. To dtermine a possible contribution to the debate from the point of view of writing materials, we used otpical and electron microscopy, various X-ray based techniques as well as vibratiional sprectroscopy. We validated our approach with SY - based studies using the advantages of the synchroton radiation source with respect to the benchtop devices. Our laboratory studies showed that often production and storage locality could be distinguished thenks to the specific residues ("fingerprint") they left on the material. Moreover, we have diescovered that diferrent parchment production processses coexisted in the antiquity, and the resulting writing materials can readily be distinguished.
Typology of Inks
Archives and museums around the world contain a vast number of manuscripts that were written in different inks: carbon inks, plant inks, iron-gall inks and mixed inks. Yet most archaeometric studies of manuscripts focus on the palette of pigments found in illuminated manuscripts whereas identification of the inks is still largely based on cultural-historical studies and visual inspections. One of the reasons of this disproportion in the studies can be explained by the properties of Raman spectroscopy, the technique of choice for identification of pigments. In contrast, this technique is only partially viable when dealing with organic colourants. Brown and Clark discuss these difficulties and the uncertainties of identification of iron-gall inks by Raman spectroscopy in their pioneering work on early medieval Anglo-Saxon manuscripts (K. Brown and R. Clark 2004). To facilitate instrumental analysis of inks, we have developed a protocol that starts with the identification of the inks type (Rabin et al. 2012) which doesn’t require complicated instrumentation and can be carried out by paleographers and codicologists.
Three typological ink classes
The black writing materials used in manuscript production in Antiquity und Middle Ages can be sorted in three typologically different ink classes: soot, plant and iron-gall. Soot ink is a fine dispersion of carbon pigments in a water soluble binding agent; plant-based ink consists of a solution of the tannins extracted from gallnuts or tree bark; iron-gall ink, is produced by mixing a soluble compound of iron (II) with gallic or tannic acid extracted from gallnuts or tree bark. Therefore, iron-gall ink presents a boundary case between solution and dispersion ink, in which a water-soluble preliminary stage oxidizes and evolves into a black, insoluble precipitate similar to the carbon pigments when the writing is exposed to air (Krekel 1999). The additional category of mixed inks, i.e. inks produced by addition of various metals to the soot inks or intentional mixing of iron-gall and soot - based inks started attracting scholarly attention only recently because their significance was established only a short while ago (Brun et al. 2016, Colini 2018, Nehring et al. 2021). We suggest that plant and mixed inks build a bridge from the carbon ink of Antiquity to the properly formulated iron-gall ink that became a standard black ink from the late Middle Ages to the 19th century when it gave way to modern inks.
Sehr geehrte Damen und Herren,
liebe Leserinnen und Leser,
bereits im ersten Band der N.i.Ke. Schriftenreihe des Netzwerks zur interdisziplinären Kulturerhaltung hatte ich angeführt, dass bei der Untersuchung von kulturellen Artefakten naturwissenschaftliche Untersuchungsmethoden zunehmend an Bedeutung gewinnen, sie eigentlich unverzichtbar geworden sind.
Ein besonders einprägsames Beispiel dieser fächerübergreifenden Zusammenarbeit zwischen Geisteswissenschaften, Naturwissenschaften und Restaurierungswissenschaften war die Ausstellung Johannes Vermeer. Vom Innehalten, die in diesem Jahr in der Gemäldegalerie Alter Meister in den staatlichen Kunstsammlungen Dresden gezeigt wurde. Eigens für diese Ausstellung wurde das Gemälde Brieflesendes Mädchen am offenen Fenster einer grundlegenden Restaurierung unterzogen. Diese Restaurierung diente jedoch nicht nur der Reparatur des Bildes. Um sich dem ursprünglichen Zustand des Gemäldes zwischen 1657 und 1659 anzunähern, wurden später hinzugefügte Malschichten großflächig abgenommen. Möglich wurde dies durch unterschiedliche, bildgebende materialwissenschaftliche Untersuchungen im Vorfeld, welche die wissenschaftlichen Grundlagen für die Diskussion über den weiteren Umgang mit der Lesenden schufen.
Materialanalytische Verfahren wurden und werden ständig weiterentwickelt und optimiert. Sei es, um aus einer Vielzahl von Einzelmessungen ein Gesamtbild zu erstellen, oder die Größe einer Probenentnahme so zu reduzieren, dass von einer „minimal-invasiven“ oder „quasi nicht-invasiven“ Untersuchung ausgegangen werden kann. Nun feiert die Bundesanstalt für Materialforschung und -prüfung, zusammen mit ihren Vorgängerinstitutionen, den königlichen Versuchsanstalten, in diesem Jahr ihren einhundertfünfzigsten Geburtstag. Sie blickt damit auf eine lange Tradition materialwissenschaftlicher Analysen zurück, an deren Beginn beispielsweise die metallographischen Untersuchungen von Adolf Martens stehen. Derartige Untersuchungen bilden auch heute noch einen wesentlichen Bestandteil archäometallurgischer Forschung. Die Historie bzw. die Weiterentwicklung der Methodik lässt sich hier besonders gut nachzeichnen. Jedoch blicken auch Verfahren zur Charakterisierung weiterer Werkstoffe, wie Glas, Keramik, oder organischer Materialien auf eine lange Geschichte zurück.
Die in diesem Band der N.i.Ke.-Schriftenreihe präsentierten Beiträge dokumentieren einerseits aktuelle Forschungsarbeiten, die erst in diesem Jahr in entsprechenden Fachjournalen publiziert wurden, andererseits liegen einige der Arbeiten bereits 50 Jahre zurück. Sie bekunden damit nicht nur die materialtechnologische und historische Bandbreite der Projekte, sondern offenbaren die Vielfältigkeit kulturhistorischer oder restauratorischer Fragestellungen, zu deren Beantwortung natur- und materialwissenschaftliche Forschung wesentliche Beiträge liefern können.
Ich bedanke mich bei allen Kolleginnen und Kollegen, die zur Erstellung dieser dritten Ausgabe der N.i.Ke. Schriftenreihe des Netzwerks zur interdisziplinären Kulturerhaltung beigetragen haben. Ihre Aufsätze ermöglichen den Blick in die Vielfältigkeit materialwissenschaftlicher Untersuchungen im Bereich Kunst- und Kulturgut. Ich wünsche Ihnen viel Spaß auf dieser kleinen Zeitreise.
The aim of this paper is to present the productive interplay of connoisseurship and material analysis when dealing with drawings by Rembrandt – or previously attributed to him – in the collection of the Klassik Stiftung Weimar. This concerns the more precise determination of the drawing materials used and the reconstruction of the genesis of the drawings discussed. The material analysis allows us to decide whether and how Rembrandt’s inks can be used to determine authorship at all. The “material turn” in drawing studies thus intervenes in the discussion about authorship and opens up a broader production aesthetic perspective. No longer the “style” but rather the handeling becomes the decisive criterion for answering the question “Rembrandt, or not?”
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).
In this paper, we discuss the importance of scientifically investigating cultural artefacts in a non-invasive way. Taking as test case Leonardo da Vinci’s Manuscript with anatomic drawings and notes, which is stored in Weimar, we clarify fundamental steps in the chronology of this folio. By means of microscopy, infrared reflectography, UV photography, and X-ray fluorescence analysis, we were able to identify various types of sketching material and several varieties of iron gall ink. For his sketches, Leonardo used two different sketching tools, a lead pencil and a graphite pencil, as well as several types of ink for developing these sketches into drawings. With regard to ink, it is important to observe that there is no difference between the ink Leonardo used for drawing and the ink he used for writing text. Based on the materials analysed, we suggest a chronology for the creation of this unique folio.
Tuschenanalyse im P 11702
(2021)
Near-inframed reflectography and imaging X-Ray flourescence analysis reveal that carbon inks of two different compositions were used in the papyrus manuscript Berlin P 11702. in contrast with the writing ink, one of the carbon drawing inks contained a significant addition of iron. This result emphasises the need for routine instrumental ink analysis.
While studying the socio-geographic history of inks, division 4.5 of the BAM (Bundesanstalt für Materialforschung und Prüfung) together with the Centre for the Study of Manuscript Cultures in Hamburg has developed a protocol for ink analysis.
It consists of a primary screening to determine the type of the ink, and a subsequent in-depth analysis using several spectroscopic techniques. The XRF elemental analysis aims primarily at identifying and characterizing metallic components of inks. Besides the instrumental methods, the paper presents an overview of historic inks in the period of transition from carbon inks of the Antiquity to iron-gall inks commonly used in the Middle Ages.
Scientific material analysis of the elemental composition of inks from different strata of a manuscript has the potential to complement scholarly observations using palaeography and philology in reconstructing the history of the manuscript’s production, correction and repair.
There are three typologically different classes of black writing inks: soot inks consist of carbon particles.
This chapter offers observations and considerations concerning black writing inks encountered in writing supports transmitting documentary and literary texts of the late Antiquity and early Middle Ages. It discusses different types of inks, the Methods of their detection and their use in different times and geographical areas.
In the transition from carbon to iron-gall inks, the two documents from the Egyptian Museum and Papyrus Collection in Berlin with shelfmarks P 13500 and P 13501 discussed in this work present an important case. Their inks appear brownish, although they date back to the fourth and third century BCE, when carbon inks are believed to have been commonly if not exclusively used. Using imaging micro-X-ray fluorescence and infrared reflectography, we discovered that the inks in both documents contain a significant amount of copper in addition to carbon. Comparing the extant recipes for black writing inks and the experimental evidence, we suggest that these inks are a transition between the pure carbon and the iron-gall inks. Such inks may have been quite common before the production of iron-gall ink was clearly understood and established.
This work presents a spectroscopic study of metallic pigments and metal foils used in reverse glass paintings that were created between 1912 and 1954. Metallic pigments induce a notable sparkling effect by means of the lateral incidence of light, whereas metal foils enhance the gloss and create a glittering effect when the painting is viewed in reflected light. Both effects were desired features especially in modern reverse paintings on glass and applied by artists in manifold creative manner. The paper gives an overview on the composition of the metalfoils and metal pigments in 14 works as determined in situ by X-ray spectrometry. Metal foils made of tin, brass, aluminium and silver were found in nine paintings. Gold imitating Cu-Zn pigments in different hues and with various Cu/Zn net intensity ratios were recorded for six paintings. Silvery pigments were identified mainly as Al pigments, but also as Cu-Zn-Ni alloy in one case. Other uncommon metallic pigments were detected in Arlequin vindicatif (c. 1925) by Floris Jespers, who used not only Cu-Zn and Al pigments, but also brownish Cu and Cu-Zn-Sn pigments. Non-invasive diffuse reflectance infrared Fourier-transform spectroscopy (DRIFTS) was used to classify the binding media of the metallic pigments. Drying oil and natural resin probably mixed with oil were the most common binding media. A polysaccharide-based binder was found in the silvery Cu-Zn-Ni pigment of Ohne Titel (1954) by Marianne Uhlenhuth.
The Scythica Vindobonensia, the new fragments on Gothic incursions into Roman provinces in the Balkans in the middle of the third century AD that were revealed some years ago in a Greek palimpsest at the Austrian National Library in Vienna (ÖNB), are commonly considered as one of the most important additions of the last decades to the corpus of texts from classical Antiquity. Tere is a high degree of confdence among scholars in supposing that the fragments come from the lost work Scythica written in Greek by the third-century historian P. Herennius Dexippus (Δέξιππος) of Athens. The new fragments have hence also been called Dexippus Vindobonensis. In his Scythica, Dexippus recorded wars of the Romans with the Goths (and other tribes) whom he called Scythians.
The work had been hitherto known only from excerpts and quotes by later authors. Eight pages of a Byzantine manuscript copy of the ancient text have survived hidden underneath the visible surface of the last four parchment folios of the Vienna manuscript Historicus graecus 73, f. 192r -195v4. The copy is written in a Greek calligraphic minuscule which has been estimated by palaeographers to be of the middle or the second half of the eleventh century. In the thirteenth century, the text (on each of the eight pages arranged in one column, with 30 lines per page) was washed of the parchment and the valuable material made from animal skin was re-used for Christian texts. The new writing largely covered the faded remnants of the original text. It thus became hidden from the human eye for more than seven hundred years. Its discovery by Jana Grusková, a classical philologist specialized in the transmission of Greek texts, resulted from a systematic review of all Greek palimpsests kept at the Austrian National Library in Vienna at the beginning of the twenty-first century and a detailed examination of the four folios in 2007-20097.
The scribe of ‘Erfurt 7’, a thirteenth-century Torah scroll now kept in Berlin, initially left blank spaces for the divine appellations Elohim ( אלהים ) and YHWH Elohim ( ,(יהוה אלהים which were filled in during a second stage of writing. The appearance of the ink employed to write the appellations was significantly darker than that of the surrounding ink.
X-ray fluorescence analysis (XRF) has shown that the light and dark brown inks had similar elemental compositions, but contained different ratios of iron to potassium, which could be explained by the use of different batches of ink.
According to some medieval sources, the divine appellations were sometimes filled in during a second stage of writing in the presence of ten men from the Jewish community. In Erfurt 7, the two-stage procedure was only performed in the first 1.5 columns of the original sheets, suggesting it may have been part of a public ceremony inaugurating the writing of the divine names in the scroll. Erfurt 7 emerges from this study not only as a ritual object used for liturgy, but as a rallying point for the Jews of Erfurt to come together as a community to express their reverence for the written form of God’s name. The divine name YHWH ( יהוה ) was written in a smaller script than the surrounding text on three replacement sheets using the same two-stage procedure. The ink used on the replacement sheets contained zinc, which is characteristic of other Erfurt manuscripts as well. This suggests that Erfurt was the place where the scroll was used, cherished and eventually repaired.
The paper presents the results of the radiocarbon dating and ink analysis of a leather fragment bearing an important liturgical text in Hebrew from the early centuries of the common era. The work initiated by the scholarly interest in the text stresses the importance of the date and materiality of the manuscripts and closes with an appeal to the curators of manuscript collections.
This thesis addresses the development of a methodological approach for the non-invasive identification of colourants and for the classification of binding media in reverse glass paintings from the early 20th century. For this purpose, mobile and miniaturized devices were used to measure the paintings in situ. The methodology includes X-ray fluorescence (XRF), VIS spectroscopy (VIS), Raman spectroscopy and diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS). In a first step the capabilities of DRIFTS for binding media classification and pigment identification were tested.
DRIFTS enables, besides Raman spectroscopy, the collection of molecular information of a substance that can be used as characteristic fingerprint spectrum. However, the simultaneous collection of both specular (surface) and diffuse (volume) reflection leads to complicated mixed DRIFT spectra, that can vary strongly for one substance depending on the dominant fraction of reflected light. Specular reflection causes several spectral distortions like inverted bands, band shifts and derivative-like features whereas pure diffuse reflections leads to an intensity enhancement of combination bands and overtones. Both specular and diffuse reflection cannot be optically separated, and their proportion depends on material properties like the absorption coefficient and the refractive index as well as on Parameters like surface roughness, porosity, grain size and angle of incidence and detection. A direct comparison of DRIFT spectra with IR spectra of other methods (e.g. transmission, ATR) is not possible, hence the creation of DRIFTS databases was needed. The next step was the complimentary utilization of Raman spectroscopy and DRIFTS for the dentification of synthetic organic colourants. Such colourants are in the further chapters called synthetic organic pigments (SOP) even when it’s not always entirely clear if they are soluble dyes or pigments that are practically insoluble in the medium in which they are incorporated. Raman spectroscopy is generally the method of choice when dealing with SOP, but fluorescence can hamper the Raman spectrum severely, inhibiting the proper identification of the pigment.
DRIFTS was successfully applied and several SOP like synthetic alizarin (PR83), the yellow azo pigments (e.g. PY1) or the red and orange β-naphthol pigments (e.g. PR3) could be identified in the paintings solely by means of DRIFTS. The holistic methodological sequence was defined after the successful establishment of DRIFTS as serious analytical alternative. As the time is always the most limiting factor for in situ measurement campaigns in museums, the 9
sequence needs to be time saving but also efficient. The methodology starts with quick measurements by XRF and VIS to get a first idea of the pigment composition, followed by the validation of the results with the vibrational spectroscopies for selected points.
Measurements of reverse glass paintings by Carlo Mense and Wassily Kandinsky were conducted to test the entire procedure. A high number of pigments could be identified, including several rare ones like strontium white (SrSO4), PR60 and PB52. The binding media were classified using the previously recorded references. The results were set in the art historian context and were discussed in a multidisciplinary way. The influence of Asian art, especially of Chinese reverse glass paintings as source of inspiration for artists of the “Blauer Reiter” collective (e.g. Wassily Kandinsky, Gabriele Münter, Franz Marc und Heinrich Campendonk) is shown. Non-invasive measurements of two Chinese reverse glass paintings from the late 19th and early 20th century were conducted, enabling a comparison of the palettes of Chinese and European painters. The Chinese palette includes heavy use of red lead and orpiment, pigments that were hardly sed in Europe anymore. More modern pigments like zinc white, cadmium yellow, viridian, chromates, cobalt blues or SOP were not found at all in the Chinese paintings.
Recent research has suggested that some of the inks used in Herculaneum papyri do not consist of pure carbon. Starting from this finding, in June 2018 a preliminary campaign of analysis by means of X-Ray fluorescence (XRF) of external portions removed mechanically from their original rolls in the eighteenth century (the so-called scorze) took place at the Biblioteca Nazionale at Naples. Also in this case, the aim of the survey was to investigate the ink composition in order to detect possible traces of metal. This article sums up the results of this survey.
The Montserrat Codex Miscellaneus (TM 59453/LDAB 552) has been the subject of numerous studies since the publication of ist first text by its owner, father Ramon Roca-Puig. Scholars have dealt with the content of its texts, as well as interrogated its origin and materiality. It is a fourth-century papyrus single quire codex, which contains texts in both Latin and Greek. It has been argued that it belonged to the Bodmer library, connected to a Pachomian library in the Thebaid. In this paper we want to contribute to the material study of the codex by presenting the first results of an archaeometric analysis performed upon the inks. The Analysis was carried out within the framework of the ‘PAThs’ project based at Sapienza University of Rome, and executed with the close cooperation of DVCTVS, a team of scholars who curate the Roca-Puig collection. The results obtained have not only cast light on the history of production of the codex, but also, and perhaps most importantly, point out that a meaningful interpretation of the analytical data is only possible through an interdisciplinary collaboration between the humanities and the natural sciences.
An interdisciplinary approach to the study of manuscript traditions is here applied to the analysis of the leaves from the White Monastery, one of the greatest centres of literary production in Late Antique Egypt. In the framework of the ‘PAThs’ project, archaeometric analyses complement the information pieced together by a range of disciplines in the field of humanities. The use of different complementary analytical techniques provides information on the type of ink used and its elemental composition, unveiling interesting details regarding the materials and methodology of manufacturing of writing media. Moreover, this contribution takes a step forward and discusses the possible existence of a regional arrangement in the elemental composition revealed in the inks studied.
Eine Vielzahl unterschiedlicher Materialien findet für die farbliche Gestaltung von Zeichnungen Verwendung. Einige Pigmente und Farbstoffe, d.h. Tinten, Stifte oder Kreiden, waren nur für den Gebrauch als Zeichenmittel vorgesehen – andere wiederum finden sich auch in der Tafel- oder Fassmalerei. Ausgehend von schwarzen Zeichenmaterialien soll zunächst eine allgemeine Typologie der Farbmittel entwickelt werden, um den Kosmos dieser Vielfältigkeit zu illustrieren. In einem zweiten Teil werden farbige Elemente am Beispiel von Rötel in Zeichnungen hinterfragt, deren Funktion und Bedeutung sich aus der Betrachtung heraus nicht unbedingt sofort erschließt. So diente die Farbe hier weder der naturgetreuen Nachahmung, noch wurde sie für eine nachträgliche Wertsteigerung eingesetzt. Der dritte Teil dieses Exkurses widmet sich schließlich solchen „farbigen“ Elementen, deren Konnotationen sich aus den Zeichnungen nicht ermitteln lassen und die daher zunächst irritieren. Diese vermeintliche Farbigkeit war aber ursprünglich vielleicht gar nicht intendiert, sondern ist vielmehr auf Alterungs- und Korrosionsprozesse zurückzuführen.
Wasserzeichen und Papierstrukturen können einen wesentlichen Beitrag bei der Analyse von Kunstobjekten auf Papier darstellen. Ausgangspunkt hierfür bildet die korrekte Dokumentation mit entsprechender Bildaufnahme und der richtigen Erfassung und Interpretation der Phänomene. An Fallbeispielen aus Forschungsprojekten zu niederländischen Zeichnungen am Kupferstich-Kabinett Dresden und der Grafischen Sammlung Weimar sollen die Möglichkeiten der Papier- und Wasserzeichenforschung als historische Hilfswissenschaft demonstriert werden. Dieser Abendvortrag dient zugleich als Einführung in die Technologie der (Hand-)Papierherstellung, Wasserzeichenerfassung und –recherche.
The aim of the lecture is to present the productive interplay of connoisseurs and material analysis using the example of selected drawings from the Rembrandt collection of the Klassik Stiftung Weimar. We try to determine the point at which the question of the materiality of the drawings makes sense in the traditional discourse of connoisseurship. On the one hand, this involves the question of authorship – Rembrandt – or not? – and the locating of attributed drawings in the context of the work. On the other hand, it is about making drawing processes visible, characterizing ways of drawing and workshop practices as well as distinguishing different forms of reworking and copying within the Rembrandt workshop. The material analyses culminate in the question of whether Rembrandt’s inks can be distinguished at all.
It becomes apparent that the newly gained knowledge about the materiality of the drawing no longer reveals itself to the “mere” view of the connoisseur. Rather, it is only generated by the digital image. The rhetoric of connoisseurs must therefore be contrasted with the necessity of a hermeneutics of the digital image. The envisaged “material turn” of drawing science is thus simultaneously able to take up the critique of the question of authorship, which has been growing ever more recently, and to transfer it to a more comprehensive perspective of aesthetics of production.
We present here our methodological approach applied to the study of Egyptian inks in Late Antiquity. It is based on an interdisciplinary strategy, bringing together a variety of disciplines from humanities and natural sciences, and it aims at systematically collecting a statistically relevant amount of data regarding the composition of the inks. The application of a wellestablished, non-invasive protocol that includes near-infrared imaging and X-ray fluorescence spectroscopy for in situ measurements enables the identification and characterisation of inks dating from the end of Late Antiquity onwards. However, sometimes this method limits our understanding when characterising more ancient inks. Trying to overcome these limitations, the potential of a new device for the characterisation of organic compounds is here explored by conducting preliminary tests on mock samples.
In this work, we present the results from 77 codicological units that include some of the earliest manuscripts of our corpus that presently lists 159 units.
In the last decade, applications of X-rays to the study of manuscripts significantly spread in both diversity and extent. They range from writing material analysis, mostly with X-ray fluorescence (XRF), permitting non-invasive characterization of inks and pigments used, to the investigation of the origin of writing supports. In addition, XRF mapping has proved to be an invaluable tool for recovering erased text. Finally, computed-tomography (CT) has shown potential in virtually unrolling rolls, making text readable without using-damaging mechanical methods. Despite their growing use, little attention has been paid to the side effects of such analytical tools. We observed irreversible parchment colour changes during some experiments on dead-sea scrolls with synchrotron radiation sources. Furthermore, partial photo-reduction of iron under high intensity beam during X-ray absorption near edge structure spectroscopy (XANES) measurements of iron-gall ink on paper has been reported several times [5,6]. Such phenomena have mostly been overlooked so far, although there is an increasing awareness of the necessity to study them. We conducted experiments at the Deutsches Elektronen-Synchrotron (DESY) facilities to investigate X-ray induced structural alteration of paper and parchment to see whether the presence of absorption centres (ink and pigments) has an impact. In addition to better understanding degradation processes, we are aiming to define an appropriate methodology of analysis of manuscripts with a tolerable risk of damage. The first results concerning X-ray induced damage of cellulose materials have already been presented at the Synchrotron Radiation and Neutrons in Art and Archaeology (SR2A). We are focusing here on the results on parchment materials.
Scientific analysis based on spectroscopic methods provide essential information on the composition of colourants and binders in paintings. These results can be set in a historical context and help to confirm art historical interpretations. Proofs of certain pigments can be used for dating purposes and may reveal if the artist used not only local but also imported materials. A pilot study of two Chinese reverse glass paintings from the late 19th (Yingying and Hongniang) and early 20th centuries (The Archer) was performed using a multi-analytical approach including X-ray fluorescence (XRF), diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and Raman spectroscopy. This approach allowed the identification of the pigments and the classification of the binding media. The results reveal a combined use of traditional Chinese and imported European materials. Several pigments like cinnabar, lead white, orpiment, carbon black and copper-arsenic green (probably emerald green) were found in both paintings; red lead, artificial ultramarine blue, Prussian blue and ochre appear in at least one of the paintings. The proof of limewash (calcite and small amounts of portlandite) as a backing layer in “Yingying and Hongniang” indicates that clamshell white was also used for reverse glass paintings. Drying oil was classified as a binding media in most areas of both paintings. However, the orange background of The Archer yielded prominent bands of both proteinaceous and fatty binder.
This paper addresses the sensitive issue of authenticating unprovenanced manuscripts of high monetary value to certify they are genuine. Over the last decade, the popularity of material studies of manuscripts using non-destructive testing (NDT) has increased enormously. These studies are held in especially high esteem in the case of suspicious writings due to the methodological rigour they are reputed to contribute to debate. We would like to stress that materials analysis alone cannot prove that an object is genuine. Unfortunately, audiences with a humanities background often tend to disregard the technical details and treat any published interpretation of instrumental analysis as an objective finding. Four examples are outlined here to illustrate what questionable contributions the natural sciences can make in describing manuscripts that have actually been forged.
Museums worldwide are equipped with different display cases. Exhibit display cases should protect cultural objects from dust as well as from mechanical and physical damage. To ensure a stable climate inside the display cases, a low air exchange rate is maintained. Typically, air exchange rates are often smaller than 0.1 d-1, which can result in rising concentrations of potential harmful VOC inside of the display cases due to emissions from materials. Especially organic acids, e. g. formic or acetic acid which can emit from e.g. sealing materials or wood-based materials, can produce damage of cultural objects.
In 2012 BAM introduced a procedure which is called: BEMMA-Scheme (Bewertung von Emissionen aus Materialien für Museums¬ausstattungen) which stands for: “Assessment of Emissions from Materials for Museum Equipment”. Regarding the testing procedure only construction materials were evaluated, not the display cases their self. Micro chambers are used for VOC emission tests of display case construction materials, e.g. plastics, sealing materials, coatings, textiles and others. Each sampling procedure is carried out in duplicate. Emissions like formic acid, acetic acid, formaldehyde, piperidine-derivates and oximes are excluded and the sum of emissions of VVOCs, VOCs and SVOCs is limited. For a positive assessment all listed criteria must be fulfilled; otherwise the display construction material fails the BEMMA scheme.
While studying the socio-geographic history of inks, division 4.5 (Analysis of cultural artefacts and assets) of the BAM (Bundesanstalt für Materialforschung und -prüfung) in Berlin together with the Centre for the Study of Manuscript Cultures in Hamburg has developed a protocol for ink analysis. It consists of a primary screening to determine the type of the ink, and a subsequent in-depth analysis using several spectroscopic techniques.
Using this protocol, scientists can assist scholars in addressing a rather broad range of historical questions that cannot be answered unequivocally through scholarly research alone. Among these are investigations on collaboration between scribes and scriptoria, on the usage and annotation of manuscripts and on their path through time and space in general. This research can thus help to reconstruct the circumstances of the production of written heritage as well as their history and transmission.
To facilitate the dialogue between the scholars and the scientists a simple optical tool was developed to allow the scholars to perform preliminary ink analysis required for formulation of the question that in turn can be answered by scientific in-depth investigations. In this paper, ink types and their identification method is accompanied by examples of the recent work conducted on parchment manuscripts in the Austrian National Library.
In the recent years multispectral imaging and X-ray Fluorescence element mapping have established themselves as a well working two step approach, when dealing with faded, erased or overwritten text in iron gall ink. During the last years a lot was done to improve the mere technical side of the techniques. Especially in the case of XRF mapping experiments the acquisition speed needed to be increased to allow mapping in the high resolution demanded by the challenges at hand. High resolution in moderate times can now be achieved, but with the price of proportionally increased amount of data that needs to be processed ideally in parallel to the measurement. The classical approach in XRF spectroscopy of elemental fitting of the spectral data does not even come close to fulfill any on the fly processing time constraints and will consume too much processing time in the foreseeable future. In this paper we will discuss the applicability of modern statistical data processing methods to XRF mapping of iron gall ink palimpsests. We will present a comparison of a new approach based on principle and independent component analysis (PCA and ICA) and the standard element mapping method. We will show that a reduction in processing time of almost two orders of magnitude can easily be achieved.
VIS-Spectroscopy of Aztec colors. Possible application of a non-destructive analytical method
(2020)
VIS-spectrometry is a rapid, non- invasive, mobile method that offers a first overview of possible colorants used for painting. This is worked out in detail for European paintings and applied for artefacts and illuminated manuscripts. Manuscripts from Asia for example show colorful decoration identified to be mostly prepared with mineral pigments such as cinnabar, azurite, malachite or orpiment, which can be well confirmed by elemental analyses due to their color-giving metal ions. This is not the case for the colorants used in pictorial manuscripts from pre-Hispanic America, painted mainly with organic dyes from plants. The palette of colors used by the Aztecs is very rich due to their extensive empire and long- distance communication with vassal states liable to tributes including dyes of high quality. These include for example red cochineal, yellow zacatlaxcalli, tagetes, safflower, and achiotl, as well as blue indigo, or matlalli.
The manuscripts – which have been inventoried as Manuscripta Americana in the State Library of Berlin and the Biblioteka Jagellońska in Krakow with the signatures Ms. Americ. 1-15 – are codices mainly from the colonial times of the 16th to 18th centuries. They uniquely reflect the relationships between indigenous culture and Spanish colonial masters. This study focusses on the scientific investigation of three manuscripts (Manuscripta Americana 3, 8, and 10) that are kept today in Krakow. It is assumed that these three parts belong together in a certain way, so various material analyses were carried out to prove this assumption. The scientific investigation focusses on the different black and brown writing inks.
At the end of the sixteenth century, a number of relics and artefacts were discovered in Granada, Spain. They included what became known as the Lead Books of the Sacromonte, twenty-one written artefacts made of circular lead leaves engraved in archaic Arabic characters. The authorship was attributed to some Arab disciples of St James the Greater considered to be the first evangelisers of the Iberian Peninsula. The texts, the materiality and the circumstances of the discoveries fuelled a debate surrounding their authenticity that lasted more than two centuries, a debate so fierce and controversial that not even papal condemnation in 1682 was able to stop it. Soon after the discoveries were made public, scholars highlighted the many contradictions and errors of a historical, linguistic and theological nature present in the texts, identifying members of the local Morisco community as possible forgers. This article focuses on how the scholarly community of the sixteenth and seventeenth centuries handled these findings and looks at the methods employed by the scholars to evaluate the authenticity of the artefacts. It will also look at how the particular interests of the various authorities involved influenced the acceptance or dismissal of relevant academic results.
Museumsvitrinen sollen Kunst- und Kulturgut „ins rechte Licht“ setzen und vor Diebstahl oder Vandalismus schützen. Vergleicht man historische Schauvitrinen, die zumeist aus einfachen Glasscheiben in Holzrahmungen bestehen, mit heutigen Konstruktionen, lässt sich eine Entwicklung zu hochtechnisierten Gebilden ablesen, die deutlich mehr Ansprüchen genügen müssen als in der Vergangenheit.
Zahlreiche Beispiele verdeutlichen, dass Kunstwerke nicht nur außerhalb, sondern auch innerhalb von Museen oder Archiven ungünstigen Umwelteinflüssen ausgesetzt sind. So können Einbauten bzw. Dekorationen in Ausstellungsräumen, Aufbewahrungsbehältnisse in Depoträumen oder Ausstellungsvitrinen flüchtige Substanzen, sogenannte VOCs (Volatile Organic Compounds) freisetzen, die zu irreversiblen Veränderungen an den Objekten führen und diese schädigen. Hierzu zählen organische Säuren, wie Ameisen- oder Essigsäure, aber auch Verbindungen, die Sulfide enthalten. Hier wird die an der BAM entwickelte BEMMA-Bewertungsmethode vorgestellt, die von Museen verwendet werden kann Materialien mit einem geringeren Emissionspotential auszusuchen.
While studying the history of inks, division 4.5 of the BAM (Bundesanstalt für Materialforschung und Prüfung) together with the Centre for the Study of Manuscript Cultures in Hamburg has developed a protocol for ink analysis. It consists of a primary screening to determine the type of the ink, and a subsequent in-depth analysis using several spectroscopic techniques. One of them, X-ray Fluorescence (XRF) aims primarily at establishing the fingerprints of inks containing metals, making it possible to distinguish among different inks.
Our research aims primarily at recreating a socio-geographic history of inks, parchment, and papyrus and includes the comparative analysis of the writing materials of the Dead Sea Scrolls, ink and papyrus in Ancient and Hellenistic Egypt, and inks in documents from various contemporary medieval communities in Fustat (first nucleus of Cairo) as well as other medieval Jewish and Armenian communities.
The presentation shows the panorama of historic inks and our attempt to follow up the transition of the inks from those based on soot to the iron-gall inks commonly used in the Middle Age.
Our study is dedicated to non-destructive characterization of the support and the inks of the DSS.
To that aim we use micro-XRF, 3D- SY-XRF, different IR methods including synchrotron radiation based reflectance spectroscopy, optical and electron microscopy.
The lecture discusses advantages and the shortcomings of the non-destructive testing approach.
The investigation of physical properties and chemical composition generates data important for answering cultural-historical questions that cannot be solved by historical and philological methods alone. Due to technological developments, technical diagnostics in art and culture are in ever-greater demand in such fields of transdisciplinary research. Natural sciences play auxiliary role in the studies of manuscripts. The success of their contribution depends strongly on the formulation of the question, the choice of the methods to obtain the requested answer, and appropriate reference databases. First, report was given on the measurements performed on local raw materials, such as, plants, minerals and animals, which constitute the reference session. Then, the first results of the scientific analysis of several fragments from the Malian manuscript collections were present.
Heute stimmen die meisten Gelehrten und Historiker darin überein, dass die Höhlen von Qumran eine Essener-Bibliothek beherberg-ten. Über ihren Ursprung, sowie die Herkunft der einzelnen Schriften, wird noch immer rege debattiert. Der aktuelle Beitrag präsentiert detaillierte Lösungsansätze zu Klärung der Provenienzfrage der Schriftrollen von Qumran.
Our research aims primarily at recreating a socio-geographic history of inks, parchment, and papyrus and includes the comparative analysis of the writing materials of the Dead Sea Scrolls, ink and papyrus in Ancient and Hellenistic Egypt, and inks in documents from various contemporary medieval communities in Fustat (first nucleus of Cairo) as well as other medieval Jewish and Armenian communities.
The presentation shows the panorama of historic inks and our attempt to follow up the transition of the inks from those based on soot to the iron-gall inks commonly used in the Middle Age.
While studying the socio-geographic history of inks, division 4.5 of the Bundesanstalt für Materialforschung und Prüfung (BAM) together with the Centre for the Study of Manuscript Cultures (CSMC) in Hamburg has developed a non-invasive protocol for ink analysis. It consists of a primary reflectographic screening to determine the type of the ink (soot, tannin or iron-gall) and a subsequent in-depth analysis using several spectroscopic techniques: X-ray fluorescence (XRF), Infrared and Raman spectroscopies. The first of them, XRF elemental analysis aims at establishing the unique fingerprints of inks containing metals or trace elements in carbon inks. In addition, we use Raman analysis to identify so-called mixed inks, an ink category that received little attention so far. Finally, with the help of IR spectroscopy we obtain information about the ink binders.
The evolution and socio-geographic distribution of writing inks from Late Antiquity to the Middle Ages are one of the foci of our investigative work at the Bundesanstalt für Materialforschung und -prüfung (BAM) in Berlin and the Centre for the Study of Manuscript Cultures, Hamburg University.
This presentation will examine the inks used by Jews in the in different geographical zones try to correlate the results of the material analysis with written records and existing traditions. We will compare the inks proposed by Maimonides, who lived in 12th-century Egypt, with the considerations of Rashi, who lived in 11th-century northern France, and see that they both advocated use of the inks commonly known and produced in their respective regions. It is Maimonides who proposes to add tannins to the soot inks, but rejects the metallic salt, both of which were practices that were well attested in contemporary Arabic recipes for making ink. In contrast, Rashi was favourable to employing the plant inks in use in contemporary Northern Europe.
Natural sciences play auxiliary role in the studies of manuscripts. The success of their contribution depends strongly on the formulation of the question and the choice of the methods to obtain the requested answer. Therefore, one should try to go beyond the understanding of the basic principles of the scientific analysis.
We will start with a glance at the basic principles of the techniques used in the material science for determination of the elemental composition (X-ray emission) and molecular composition (FTIR & Raman). We will move then to the bench and mobile equipment commonly used in the field of cultural heritage. At the end we will choose a question to be answered and design an ideal experiment that will be modified according to the limitations dictated by on-site conditions.
In the ateliers in the afternoon we will
a) compare two XRF devices that differ in their spatial resolution;
b) use a high resolution microscope (Keyence) to obtain a close look at writing surfaces and materials;
c) we will learn to determine the type of the inks with the help of another microscope (DinoLite AD413T-12V), a usb microscope with visible, UV and NIR illumination;
d) we will learn to use FTIR-ATR device for determination of the type of the writing surface;
e) We will use mobile Raman device for identification of pigments.
Parchment
(2019)
This lecture will present history of parchment based on written sources and chemical examination of antique, medieval and modern parchment.
Our studies of the Dead Sea Scrolls writing surfaces show that they can be divided roughly into three groups: leather, parchments of a light tint, and those of various shades of brown. The latter ones are invariably tanned, whereas the middle group is characterized by the presence of various inorganic salts. Some of the pale parchments, among them the Temple Scroll (11Q19), are remarkably similar to medieval European parchment. Therefore we have formulated the working theory that in the Judaea of the Hellenistic period two different parchment-making traditions existed side by side: an ‘eastern’ one (represented by the tanned parchments of Qumran, closely resembling Aramaic documents from the fifth century BC, and a ‘western’ one (represented by the untanned/lightly tanned ones similar to early Christian Greek parchments).
This division has found support during our studies of the Geniza fragments, in which Babylonian and Palestinian traditions seem to follow the “eastern” and “western” technologies, respectively.
Inks and pigments
(2019)
The writing materials used in various cultures and epochs can be divided into two groups. The first comprises materials that write themselves, producing script by rubbing their own material off onto the writing surface. It includes charcoal, graphite, chalk, raddle, and metal styluses. Depending on the material and consistency, these are cut or pressed to make styluses and then used for writing.
The second group comprises all coloring liquids that are applied to the writing surface with a quill, pen, or printing block. It includes inks made from dye solutions (for example, tannin inks) and those made from pigment dispersions (for example, sepia, soot, and bister inks). The latter are sometimes also rubbed as pastes into letters incised into the writing surface, where they increase visual contrast.
Due to the variety of recipes and the natural origin of raw materials, there is a wide range of different components and impurities in writing materials.
Soluble inks (Tinten)
Soluble inks are based mainly on dyes forming a water solution. Colored inks were manufactured with different plant or insect dyes (e.g. Brazil wood, kermes). To stabilize the volatile material, the dyes were mixed with a mordant (e.g., alum).
Brown plant inks – best-known as blackthorn or Theophilus’ inks – are usually produced from the blackthorn bark and wine. In the early European Middle Ages, inks of this kind were widely used in the production of manuscripts in monasteries. Usually, they are light brown, so sometimes small amounts of iron sulfate were added, which led to what was called an “imperfect” iron gall ink. The difference between “classic” iron gall ink and such imperfect ink is therefore not clear: the distinction is not possible, especially with the naked eye.
Dispersion inks (Tuschen)
According to its generic recipe, one of the oldest black writing materials is produced by mixing soot with a binder dissolved in a small amount of water. Thus, along with soot, binders such as gum arabic (ancient Egypt) or animal glue (China) are among the main components of soot inks. From Pliny’s detailed account of the manufacture of various soot-based inks, we learn that, despite its seeming simplicity, producing pure soot of high quality was not an easy task in Antiquity. Therefore, we expect to find various detectable additives that might be indicative of the time and place of production. One such carbon ink requires the addition of copper sulfate . The experimental discovery of this ink in 1990 led to a misleading expression “metal ink” that is sometimes found in the literature.
Colored dispersion inks based on pigments such as orpiment, cinnabar, or azurite have been known since Antiquity. Natural or artificially produced minerals are finely ground and dispersed in a binding medium. As in soot inks, water-soluble binders such as gum arabic or egg white were used.
Iron gall ink (Eisengallustinten)
Iron gall inks are a borderline case between these two groups. They are produced from four basic ingredients: galls, vitriol as the main source of iron, gum arabic as a binding media, and an aqueous medium such as wine, beer, or vinegar. By mixing gallic acid with iron sulfate, a water-soluble ferrous gallate complex is formed; this product belongs to the type “soluble inks”. Due to its solubility, the ink penetrates the writing support’s surface, making it difficult to erase. Exposure to oxygen leads to the formation of insoluble black ferric gallate pigment, i.e., “dispersion ink”.
Natural vitriol consists of a varying mixture of metal sulfates. Since for ink making it was obtained from different mines and by various techniques, inks contain many other metals, like copper, aluminum, zinc, and manganese, in addition to the iron sulfate. These metals do not contribute to color formation in the ink solution, but possibly change the chemical properties of the inks.
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.
The objective of this study is to find out, to what extent the geochemical characteristics of lapis lazuli can be utilized in respect to its provenance. A wide range of variables is taken into consideration depending on the quantity of samples analysed from a specific geological region and the methods applied. In order to provide evidence, a multi-technique analytical approach using µXRF, ESEM, PGAA and PIXE is applied to samples from the most famous deposits of lapis lazuli. Special elements determined as fingerprints are compared in relation to the forming conditions obvious in textural features. The results and statistical output allow a differentiation that enables an optimized local classification of the blue stone. An absolute requirement for all geo-tracing performed on blue colored cultural objects of unknown provenance is awareness of the limits of analysis. The possible sources of lapis lazuli are tested by analysing the blue pigment used as paint on murals and ink on manuscripts from the Silk Road.
The initial focus of this research was on the development of a general workflow for the documentation and monitoring of historical stained glass windows using structured light scanning. Therefore windows from different churches, time periods and with different corrosion and damage phenomena were scanned before and after conservation measures. To evaluate the execution of the restoration measures the data was compared using 3D inspection software to examine the differences in geometry between the two scans. Various problems had to be solved, for example, how to deal with heavily reflective surfaces and the extreme contrast between light and dark surfaces, as seen in the borders between ‘Schwarzlot’ painting and plain glass. The application of materials for matting the surfaces, such as Cyclododecane spray, was impossible due to the high accuracy of the surface measurement required for 3D inspection. Regarding the contrast differences of the surfaces, the creation of exposure fusions and the use of polarization filters to reduce reflections were tested. In addition to the general problems encountered when recording translucent surfaces, the historical glasses caused additional problems in calculating surface comparisons. For example, the windows have to be moved and turned around several times, both during the conservation process and while scanning, causing deformations of the geometry due to the flexible lead rods allowing a certain degree of movement.
Im Jahr 2019 jährt sich die Inbetriebnahme der ersten Papiermaschine in Deutschland zum 200. Male. Mit dem Vortrag wird eine Einführung in die Technologie der Maschinenpapierherstellung, samt entwicklungsgeschichtlicher Meilensteine gegeben. Es gilt die Produktvielfalt von Papier und die Gründe für die enormen Produktionssteigerungen bei der Papierherstellung aufzuzeigen.
Wasserzeichen und Papierstrukturen können einen wesentlichen Beitrag bei der Analyse von Kunstobjekten auf Papier darstellen. An Fallbeispielen aus der gutachterlichen Praxis und Forschungsprojekten der Vergangenheit sollen die Möglichkeiten der Papier- und Wasserzeichenforschung bei Datierungen und Authentizitätsprüfungen demonstriert werden.
The initial focus of this research was on the development of a general workflow for the documentation and monitoring of historical stained glass windows using structured light scanning.
Therefore windows from different churches, time periods and with different corrosion and damage phenomena were scanned before and after conservation measures.
In the 15th century, Persian manuscripts underwent significant and lasting changes. Possibly as a response to the import of tinted and gold-decorated paper from China, which was used for manuscript production in Greater Iran, Persian papers were also tinted and embellished with gold-decorated and marbled margins or frames. In a joint project between CSMC and the University of St Andrews, we aim to analyse papers and their decorations in Persian The analyses aim to determine the consistencies of papers, pigments and metals and the techniques used for their production and application. The support will be first described in its codicological characteristics such as dimensions, thickness, colour (expressed in colour coordinates), pattern left from the sieve (observed in transmitted light). The plant used as raw material in paper production will be studied by fibres analysis, while the sizing agents, the pigments, dyes and metals will be analysed by the application of several methods: in particular Reflectography, X-Ray Fluorescence and InfraRed, Raman and Visible Reflectance Spectroscopy. The results of the analyses will form an important resource for the material aspects of Persian manuscripts and be a starting point for establishing a first chronology of the materials and techniques used in Persian manuscript production. An example of the application of the techniques on the analysis of a fragment from a 15th c. Persian Manuscript will be provided.
Papyrus was in use in the Islamic world until the 11th century and few ink recipes collected from treatises about the art of the books are dedicated to this support. But papyrus was also burnt in order to obtain soot used as an ingredient for a particular type of ink (midād al-qarāṭīs). In this talk I will give an overview of the recipes – in particular those by ar-Rāzī –, their context and transmission in order to evaluate this double nature of papyrus, which is considered at the same time a writing support and a material to be recycled. Moreover, I will discuss what kinds of ink are most likely to be found, according to these literary sources, on Arabic manuscripts and documents written on papyrus and compare them to the typologies mentioned for paper and parchment. These results are the premises of a research project starting at the beginning of 2019, in which a number of dated fragments from several European institutions will be analysed with non-destructive techniques in order to establish a profile of the main writing media used in the early centuries of the Islamic Era.
Fifty shades of black: Typologies and terminology of black inks in the light of new discoveries
(2019)
The identification of the materials constituting an artefact is the basis of any correct conservation project. For this reason (among others) in the last 50 years analytical techniques have been applied to the study of manuscripts. Unfortunately, the scientific investigation of Arabic books is still uncommon, focusing mainly on single case studies of illuminated manuscripts where the black media used to write the text is largely overlooked. This lack of knowledge prompted a recent research in which black ink recipes have been collected from written Arabic sources, their feasibility has been assessed, and some of them have been reproduced. These samples were artificially aged and analysed through an array of analytical techniques, mostly non-invasive and non-destructive, in order to build a database of Arabic inks and their ingredients and to verify the detection limits of the equipment employed. Finally, the results were compared to the data collected from historical manuscripts.
In this talk I will focus on the ink typologies and the terminology (ancient and modern) used to describe them. In particular I will highlight how even the modern classification fails to capture the variety encountered in both recipes and manuscripts, particularly in the light of recent discoveries. I will address especially the terminological and conceptual issues of mixed inks – in the form of carbon inks and tannins, of carbon and iron gall inks, and of carbon and metallic salts –, iron gall inks made without vitriol and iron gall inks made with sources of tannins different from gall nuts.
Ink recipes from the islamic era: Texts, manuscripts, ink reproductions and scientific analyses
(2019)
Ink recipes can often be found in Arabic manuscripts. They may be included in treatises of diverse subjects – from handbooks for secretaries or calligraphers to books on arts and crafts, to alchemical and astrological essays. Recipes can also appear, with or without relation to the main text in the manuscript, in the form of lists or collections or even added in empty spaces as single entries. Why were these recipes written down? Were they used by the many professionals dealing with inks in their every-day work? Or were they part of the literary genre of adab with little or no practical application? To answer these questions a research project was set up: ink recipes have been collected from written Arabic sources, their feasibility has been assessed and some of them have been reproduced. These samples were artificially aged and analysed through an array of analytical techniques, most non-invasive and non-destructive, and the results compared to the data obtained by the application of the same analyses on concrete manuscripts. The codicological characteristics of the manuscripts have also been studied. My aim in this talk is to show how such an interdisciplinary approach could be beneficial for the study of material culture.
This talk will be divided into two parts. In the first part I will present the analytical techniques and the equipment used by the Centre for the Study of Manuscript Cultures that can be applied for the study of decorated papers. The analyses aim to determine the constituent materials of papers, pigments, dyes and metals and the techniques used for their production. I will focus in particular on the kind of information these techniques allow us to gather: through optical microscopy we conduct fibre analysis in order to identify the plant used as raw material in paper production while Reflectography, X-Ray Fluorescence and InfraRed, Raman and Visible Reflectance Spectroscopy are used to study the sizing agents, the pigments, dyes and metals. In the second part I will show some results obtained by the application of these techniques on a few Persianate manuscripts, dating between the 15th and 17th centuries, belonging to the corpus of Ilse Sturkenboom.
In this poster we will present some results of a research projects dealing with Arabic recipes of black inks [1-2]. To improve conservation practices of Arabic manuscripts we have assessed the feasibility of the recipes collected from many Arabic sources on bookmaking and reproduced the most common inks. Ink samples were then artificially aged and analysed using an array of analytical techniques, mostly non-invasive, in order to build a database of Arabic inks and their ingredients and also to verify the detection limits of the portable equipment employed.
We will show procedures and problems concerning the identification of ink types and ingredients using reflectography (in Vis, IR and UV), X-Ray Fluorescence, Infrared and Raman spectroscopy. The focus will be in particular on squid ink [3] and mixed inks – both in the form of carbon inks with the addition of tannins and of a mixture of carbon and iron gall inks – which are particularly difficult to detect [4]. We will also examine the results of iron gall inks made with iron filings or nails instead of vitriol, the various precursor used to extract gallic acid that are mentioned in the sources as surrogates of gall nuts.
[1] A. Schopen, Tinten und Tuschen des arabisch-islamischen Mittelalters, Göttingen: Vandenhoeck & Ruprecht, 2004
[2] S. Fani, Le arti del libro secondo le fonti arabe originali. I ricettari arabi per la fabbricazione degli inchiostri (sec. IX-XIII): loro importanza per una corretta valutazione e conservazione del patrimonio manoscritto, PhD thesis, Napoli: Università L’Orientale, 2013
[3] S. Centeno, J. Shamir Journal of Molecular Structure, 873 (2008), 149-159
[4] C. Colini et. al, Manuscript cultures, 11 (2018) 43-50
In this poster we will present some results of a research projects dealing with Arabic recipes of black inks. To improve conservation practices of Arabic manuscripts we have assessed the feasibility of the recipes collected from many Arabic sources on bookmaking and reproduced the most common inks. Ink samples were then artificially aged and analysed using an array of analytical techniques, mostly non-invasive, in order to build a database of Arabic inks and their ingredients and also to verify the detection limits of the portable equipment employed.
We will show procedures and problems concerning the identification of ink types and ingredients using reflectography (in Vis, IR and UV), X-Ray Fluorescence, Infrared and Raman spectroscopy. The focus will be in particular on squid ink and mixed inks – both in the form of carbon inks with the addition of tannins and of a mixture of carbon and iron gall inks – which are particularly difficult to detect. We will also examine the results of iron gall inks made with iron filings or nails instead of vitriol, the various precursor used to extract gallic acid that are mentioned in the sources as surrogates of gall nuts.
In the 15th century, Persian manuscripts underwent significant and lasting changes. Possibly as a response to the import of tinted and gold-decorated paper from China, which was used for manuscript production in Greater Iran, Persian papers were also tinted and embellished with gold-decorated and marbled margins or frames. In a joint project between CSMC and the University of St Andrews, and in co-operation with the Golestan Palace Museum, we aim to analyse papers and their decorations in manuscripts in the holdings of the Golestan Palace Library. The analyses aim to determine the consistencies of papers, pigments and metals and the techniques used for their production and application. The support will be first described in its codicological characteristics such as dimensions, thickness, colour (expressed in colour coordinates), pattern left from the sieve (observed in transmitted light). The plant used as raw material in paper production will be studied by fibres analysis, while the sizing agents, the pigments, dyes and metals will be analysed by the application of several methods: in particular Reflectography, X-Ray Fluorescence and InfraRed, Raman and Visible Reflectance Spectroscopy. The results of the analyses will be published in an online database that will form an important resource for the material aspects of Persian manuscripts and be a starting point for establishing a first chronology of the materials and techniques used in Persian manuscript production.
The earliest known recipes for iron gall inks include four basic ingredients: oak galls – pathological growths of oak leaves; metal salts – usually referred to as vitriol; a binder such as gum Arabic; and water. The final product differs in the elemental composition due to the multitude of recipes as well as differences within the composition of the ink’s ingredients. Nowadays, based on the qualitative and semi-quantitative evaluation of X-ray fluorescence data, it is possible to distinguish inks on the basis of the so-called fingerprint model. The first goal of our study was to determine to what extent the type of XRF spectrometer affects the quality of the ink evaluation. We tested two types of spectrometers, semi-stationary machines equipped with polycapillary focusing optics and a handheld spectrometer with a diaphragm collimator and a relatively big interaction spot.
The second goal was to address the issue of whether the ink composition might be affected by storage in a metal container. The presentation will discuss the role of the spectrometer type in the evaluation of a thin layer material such as ink.
We have also learned that the iron-gall ink composition might depend on the type of vessel in which ink was being stored.
Im Rahmen des Projektes „Hinterglasmalerei als Technik der Klassischen Moderne von 1905 – 1955“, welches vom Museum Penzberg – Sammlung Campendonk, Penzberg (Gisela Geiger und Diana Oesterle) geleitet wurde und in Zusammenarbeit mit der freischaffenden Restauratorin Simone Bretz, der Bundesanstalt für Materialforschung und -prüfung (BAM) und dem Doerner Institut erfolgte, konnte im Rahmen einer Promotion erstmals ein Konvolut von mehr als 60 Hinterglasbildern mit nicht-invasiven Analysemethoden untersucht werden. Die eingesetzten Verfahren ermöglichten die Identifizierung der Pigmente und eine Klassifizierung der verwendeten Bindemittel.
Die materialwissenschaftliche Beschäftigung mit der Hinterglaskunst in ihrer Vielfalt ist ein relativ junges Forschungsfeld. Lange wurde ihr mit Unkenntnis, Missverständnis und sogar Geringschätzung begegnet. Im kunsthistorischen Kontext wurde diese Art der Kaltmalerei zumeist mit dem Begriff der Glasmalerei belegt und nicht als eigenständige Kunstform anerkannt, da in beiden Fällen Glas als Bildträger seinen Einsatz findet. In der Hinterglasmalerei wird die Tafelrückseite mit organisch gebundenen Malfarben verziert und das Werk ausschließlich bei auffallendem Licht betrachtet. Die künstlerische Herausforderung liegt immer in der technischen Notwendigkeit eines umgekehrten Malvorganges: die oberste, durch das Glas sichtbare Schicht muss zuerst auf den Bildträger Glas aufgetragen werden, der optische Hintergrund wird zuletzt aufgebracht. Im Vergleich zum Tafelbild, bei dem die Malerei erst durch den Firnisauftrag Tiefenlicht erhält, entfalten die Farben in der Hinterglasmalerei bereits beim Malen ihre Intensität und erhalten gleichzeitig Schutz durch den gläsernen Bildträger (Bretz et al. 2016).
Neben der kunstgeschichtlichen und kunsttechnologischen Bearbeitung der Hinterglasbilder spielten materialwissenschaftliche Untersuchungen an einer Auswahl von 66 Bildern im Rahmen des von der VolkswagenStiftung finanzierten Forschungsprojektes eine zentrale Rolle. Grundsätzlich wurde ein nicht-invasiver Ansatz gewählt, um die fragilen Kunstwerke in-situ zu messen und somit einen Transport zu vermeiden. Die Methodik umfasst neben VIS-Spektrometrie in Reflexion und energiedispersiver Röntgenfluoreszenzanalyse (RFA) auch Infrarotspektroskopie in diffuser Reflexion (DRIFTS) und Raman-Spektroskopie. Mit Hilfe des gewählten methodischen Ansatzes lassen sich sowohl anorganische als auch organische Pigmente identifizieren und die Zusammensetzung von Metallfarben und Folien sowie die Glaszusammensetzung qualitativ bestimmen. Ferner ermöglicht die DRIFT-Spektroskopie eine Klassifizierung der Bindemittel.
Die im Rahmen des Forschungsprojektes analysierten Hinterglasbilder können folgendermaßen chronologisch gruppiert werden: 1910-1919 (17 Bilder), 1920-1929 (18 Bilder), 1930-1939 (6 Bilder), 1940-1949 (7 Bilder), 1950-1955 (13 Bilder) und >1955 (5 Bilder). Die Auswertung der Ergebnisse ermöglicht grundsätzliche Aussagen über die verwendeten Malmaterialien in Hinterglasbildern in der ersten Hälfte des 20. Jahrhunderts und zeigt Änderungen der verwendeten Pigmente im zeitlichen Kontext auf.
Während der ersten Hälfte des 20. Jahrhunderts kamen viele neue Pigmente und Malmaterialien auf den Markt, wobei speziell die synthetischen organischen Pigmente (SOP) zu nennen sind. Eine Vielzahl an SOP konnte in Hinterglasbildern aus allen Zeitgruppen identifiziert werden, wobei hier vor allem Farblacke aus synthetischem Alizarin (PR83), Vertreter der roten und orangen β-Naphthol Pigmente [(z.B. PR3, PR4, PO5 (in Nächtliche Fahrt, 1921 von L. Hildebrandt nachgewiesen)], die blauen und grünen Kupferphthalocyanine [z.B. PG7, PB15 (taucht ab 1949 in Hinterglasbildern auf)] und einige gelbe Azopigmente [z.B. PY1, PY3, PY12 (in Geneigter Mädchenkopf, 1941 von Oskar Schlemmer gefunden)] aufzuführen sind (Steger et al. 2018; Steger et al. 2019a). Einige seltene SOP der Triarylcarboniumgruppe konnten ebenso nachgewiesen werden. Darunter fallen neben der Identifizierung von PR81 (Ohne Titel, 1954, M. Uhlenhuth) auch die erstmaligen Nachweise von PV2 (Hahn, um 1945, L.-G. Buchheim) und PG1 (Exzellente und einmalige Dressuren, 1945/46, L.-G. Buchheim) in Kunstwerken überhaupt (Steger et al. 2018; Steger et al. 2019a). Ferner konnten mit PB52 aus der Gruppe der Anthrachinone und PR60 aus der Gruppe der verlackten Naphthalin-Sulfonsäure-Pigmente weitere seltene SOP in den Bildern Rudern (um 1912) beziehungsweise Apokalyptischer Reiter II (1914) von Wassily Kandinsky nachgewiesen werden (Steger et al. 2019b).
Neben den Entwicklungen der SOP können auch eindeutige Trends in den anorganischen Pigmenten veranschaulicht werden. Seltene anorganische Pigmente wie zum Beispiel Strontiumweiß (SrSO4) in der Kreuzabnahme (1914/15) von Carlo Mense (Steger et al. 2019c) wurden identifiziert. Neu entwickelte anorganische Pigmente wie zum Beispiel Cadmiumrot (Cd(S,Se); ab 1928 in 11 Hinterglasbildern nachgewiesen) oder Titanweiß (TiO2; Anatas kommt ab 1922 vor, Rutil konnte nur in Kissen der Träume, 1976 von Werner Schriefers identifiziert werden) tauchen in einigen Hinterglasbildern auf. Schweinfurter Grün (3Cu(AsO2)2·Cu(CH3COO)2) oder Strontiumgelb (SrCrO4) wurden in einigen Bildern bis etwa um 1925 gefunden; diese Pigmente konnten dagegen in späteren Bildern nicht mehr nachgewiesen werden. Als Beispiel sind hier vier frühe Hinterglasbilder (1909–1914) von Wassily Kandinsky zu nennen, wobei Strontiumgelb in vielen Bildpartien zu finden war (Steger et al. 2019b). Publizierte materialwissenschaftliche Ergebnisse von Kandinskys Leinwandgemälden aus späteren Werksperioden zeigen, dass Strontiumgelb zu dieser Zeit vollkommen aus seiner Palette verschwunden ist und vor allem durch ein anderes Gelbpigment, nämlich Cadmiumgelb, ersetzt wurde (McMillan et al. 2013).
Eine materialtechnische Besonderheit in der Hinterglaskunst ist die Verwendung von Metallfolien und Metalleffektpigmenten. Metallfolien aus Silber, Zinn, Aluminium oder Messing wurden vielfach als künstlerisches Element in die Komposition integriert, wobei sie als finale Schicht auf, die bereits gestaltete, leicht transparente Malerei geklebt wurden. Durch die Betrachtung im auffallenden Licht erzeugten die Folien bemerkenswerte Glitzereffekte. Zinn- und Aluminiumfolien wurden zum Beispiel in Rudern (um 1912, W. Kandinsky) nachgewiesen, während Messingfolien häufig in Bildern von L.-G. Buchheim gefunden wurden. Die Zinnfolien wurden im 19. und frühen 20. Jahrhundert für Verpackungszwecke (z.B. Zigaretten, Schokolade) verwendet. Aluminiumfolie wurde erst ab 1910 industriell in der Schweiz hergestellt und zu Beginn vor allem für Schokoladenverpackungen eingesetzt (Skrabec 2016). Die frühe Verwendung solche Folien in Hinterglasbildern (z.B. Rudern, um 1912) zeigen eine rasche Verbreitung dieses Materials bei den Künstlern an. Unter Metalleffektpigmenten versteht man feingemahlene Pulver aus Metall (z.B. Zinn, Nickel, Kupfer) und Legierungen (z.B. Messing, Neusilber) mit unterschiedlichen Tönungen, welche bei seitlichem Lichteinfall auf Hinterglasbildern ein merkbares Funkeln erzeugen. Solche Metalleffektpigmente wurden vielfach bei Werken von Heinrich Campendonk nachgewiesen (Geiger und Bretz 2017) und konnten in allen chronologischen Gruppen gefunden werden.
Grundsätzlich ermöglichen die Ergebnisse ein besseres Verständnis für die Technik der Hinterglasmalerei und helfen insbesondere, diese eigenständige Kunst im Hinblick auf die „klassische“ Tafel- bzw. Leinwandmalerei abzugrenzen. So zeigen Vergleiche mit Gemälden auf Leinwand von Wassily Kandinsky deutliche Unterschiede in den verwendeten Farbmitteln für beide Techniken. Die Anzahl von 66 gemessenen Hinterglasbildern von 39 Künstlern erscheint im Kontext von über 1200 Arbeiten, welche im Rahmen des Projektes lokalisiert werden konnten, gering. Allerdings können die durchgeführten Untersuchungen als Startpunkt für zukünftige Projekte in diesem Forschungsfeld, beispielsweise für einzelne Werkkomplexe verstanden werden.
Die Forschungsergebnisse werden auf die Webseite www.hinterglas-klassischemoderne.de eingestellt. Im Sommer 2020 präsentiert das Museum Penzberg – Sammlung Campendonk Hinterglasbilder von 1910 bis 1960 als Abschlussausstellung des Forschungsprojektes. Die Ausstellung wird von einem ausführlichen Katalog über die fächerübergreifende Forschung begleitet. Für Herbst 2020 ist ein Hinterglas-Symposium an der Bundesanstalt für Materialforschung und -prüfung (BAM) Berlin im Rahmen eines N.i.Ke. Workshops geplant.
In this poster we will present some results of a research projects dealing with Arabic recipes of black inks. To improve conservation practices of Arabic manuscripts we have assessed the feasibility of the recipes collected from many Arabic sources on bookmaking and reproduced the most common inks. Ink samples were then artificially aged and analysed using an array of analytical techniques, mostly non-invasive, in order to build a database of Arabic inks and their ingredients and also to verify the detection limits of the portable equipment employed.
First, we will provide an overview of the sources [1-2] employed in the study – dating from 9th to 14th century, although the manuscripts in which they can be found dates up to the 20th century – with an eye on the ink typologies (real and perceived by the compilers). Then we will show how, by reproducing the recipes, it was possible to shed light on some oddities in the procedures and the choice of ingredients. In the end we will discuss problems concerning the identification of ink types and ingredients using reflectography (in Vis, IR and UV), X-Ray Fluorescence, Infrared and Raman spectroscopy. The focus will be in particular on mixed inks – both in the form of carbon inks with the addition of tannins and of a mixture of carbon and iron gall inks – which are particularly difficult to detect [3]. We will also examine the results of iron gall inks made with iron filings or nails instead of vitriol and the various precursor used to extract gallic acid that are mentioned in the sources as surrogates of gall nuts.
[1] A. Schopen, Tinten und Tuschen des arabisch-islamischen Mittelalters, Göttingen: Vandenhoeck & Ruprecht, 2004
[2] S. Fani, Le arti del libro secondo le fonti arabe originali. I ricettari arabi per la fabbricazione degli inchiostri (sec. IX-XIII): loro importanza per una corretta valutazione e conservazione del patrimonio manoscritto, PhD thesis, Napoli: Università L’Orientale, 2013
[3] C. Colini et. al, Manuscript cultures, 11 (2018) 43-50