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The quest for the mixed inks
(2018)
In this article, we would like to share our observations concerning the inks produced by intentionally mixing soot or charcoal with tannin extracts or iron-gall ink. Aside from Zerdoun’s mention in her outstanding review of written sources, “Les encres noires au Moyen-Âge”, this ink category has received little if any attention from scholars and scientists. And yet, if analytically attested, the use of such inks could serve as an additional category to classify and distinguish the writing inks on the historical socio-geographic map of the writing inks we are trying to build.
The Erfurt Hebrew Giant Bible and the Experimental XRF Analysis of Ink and Plummet Composition
(2007)
The aim of our work was to check whether the assumption that the jar was discovered in Qumran can be substantiated. In order to establish the archaeological provenance of the jar we conducted a series of analytical tests on samples of material collected from the jar in April and June 2009. The samples were either found loose within the jar, these being probably constituted by remnants of its original contents, or were clay detached from the inner and outer surface of the jar. In addition, a portion of sand deposit coating the inside of the jar handles was analysed.
Ancient papyri are a written heritage of culture that flourished more than 3000 years ago in Egypt. One of the most significant collections in the world is housed in the Egyptian Museum and Papyrus Collection in Berlin, from where the samples for our investigation come. The papyrologists, curators and conservators of such collections search intensely for the analytical detail that would allow ancient papyri to be distinguished from modern fabrications, in order to detect possible forgeries, assess papyrus deterioration state, and improve the design of storage conditions and conservation methods. This has become the aim of our investigation. The samples were studied by a number of methods, including spectroscopic (FTIR, fluorescent-FS, Raman) diffractional (XRD) and chromatographic (size exclusion chromatography-SEC), selected in order to determine degradation parameters: overall oxidation of lignocellulosic material, degree of polymerization and crystallinity of cellulose. The results were correlated with those obtained from carefully selected model samples including modern papyri and paper of different composition aged at elevated temperature in humid air. The methods were classified in the order SEC > FS > FTIR > XRD, based on their effectiveness in discriminating the state of papyri degradation. However, the most trustworthy evaluation of the age of papyri samples should rely on several methods.
L'archéométrie est une discipline riche qui peut nous apporter beaucoup d'informations sur l'étude des manuscrits et qui, conjuguée à la paléographie et la codicologie, peut s'apporter un outil précieux pour mieux appréhender les sociétés qui ont produits ces manuscrits.
Nous verrons ici quelques exemples de techniques scientifiques non destructives, principalement appliqués à la Génizah du Caire, appliquées à l'étude des manuscrits.
In this study, we address the question of the
provenance and origin of the Dead Sea Scrolls manuscripts.
A characteristic low ratio of chlorine to bromine, corresponding
to that of the Dead Sea water, may serve as an indicator for
local production. For this aim we developed a non-destructive
procedure to determine the Cl/Br ratio in the parchment of
these manuscripts. Micro-X-ray fluorescence (µ-XRF) measurements
of a large number of parchment and leather
fragments from the Dead Sea Scrolls were analyzed with a
routine we developed based on fundamental parameter
quantification. This routine takes into account the absorption
of the collagen matrix and the influence of the different sample
thicknesses. To calculate the representative Cl/Br ratio for each
fragment, we investigated the lateral homogeneity and
determined the total mass deposition using the intensity of
the inelastically scattered, characteristic tube radiation. The
distribution of the Cl/Br ratios thus obtained from the µ-XRF
measurements make it possible to distinguish fragments
whose origin lies within the Dead Sea region from those
produced in other locations.
The manuscript Codex germanicus 1 (Cod. germ. 1) of the Staats- und Universitätsbibliothek Hamburg is a fifteenth-century German-language manuscript. It comprises two codicological units and has an especially complex developmental history. To trace this developmental history, neglected until now in the research literature, the manuscript was investigated, for the first time not solely with classical codicological and palaeographical methods, but also with the aid of X-ray fluorescence spectroscopy, in order to determine the composition of the writing materials. These methods made it possible, first, to support and check palaeographic findings and, second, to gain information about the stratigraphy of the manuscript where palaeographic methods find their limits – in regard to short entries, rubrications, and non-alphabetical signs.
In this study we demonstrate the possibility to identify the production area of the scrolls, coupling non-destructive quantitative analysis of race elements to spectroscopic investigation of the inks. This approach, that allowed us to determine the Dead Sea area as origin of 1QHodayot, is of general validity.
The experimental knowledge about the inks of antiquity and late antiquity rarely goes beyond their visual description. In rare cases, inks typology has been determined by means of microscopy and reflectography, i.e. using their physical and optical properties, respectively. Soot, plant, and iron gall inks form different typological classes of historical black writing materials. Soot ink is a fine dispersion of carbon pigments in a water-soluble binding agent; plant-based ink consists of tannin solution; iron gall-ink presents a boundary case between soot and plant ink— a water soluble preliminary stage (similar to inks from the second group) oxidizes and evolves into a black, insoluble material (similar to the carbon pigments of the first group) when the writing is exposed to air. Each ink class has distinct properties that would readily permit their easy differentiation, if only these historical inks always belonged to just one of the classes above. In reality, inks may contain additives that obscure a clear picture.
All the black inks of the DSS have been hitherto identified as soot inks. Yet some manuscripts, with 1QapGen ar among them, display ink corrosion that is incompatible with the pure soot ink. This type of corrosion commonly observed in medieval manuscripts written with iron gall inks, results from the catalytic action of metallic component in the ink. Early analysis of this ink conducted by Nir El and Broshi in 1996 found copper in the corrosive inks and attributed its presence to the use of bronze inkwells. Re-investigation of the 1QapGen ar ink suggests, however, that the ink composition, soot + copper, agrees well with the ink recipe recorded in the 1st century CE by Dioscorides. Similar inks have been already attested on contemporary Egyptian papyri. The first part of the paper is dedicated to the new results on the inks and corrosion pattern of the 1QapGen ar.
In the second part of the presentation I will focus on the luxury scrolls, a distinct codicological type introduced by E. Tov. Our studies show that the preparation of the writing materials cannot supplement the list of codicological criteria offered by Tov. Therefore, one can divorce the writing material production from its inscription in contrast with the medieval scriptoria practices that included parchment production and copying of the manuscripts.
The Dead Sea Scrolls belong to the most important cultural assets of mankind. Their long term preservation and study is a challenge that demands an interdisciplinary approach. As early as the 1950s natural scientists assisted the scholars in studying the scrolls. It was at this time that the first extensive study of the scroll material took place. It was found that most fragments were written not on leather but on parchment. In addition, a method for determining the age of the parchment was developed which is still of value today. In the 1990s the AMS-C14 method confirmed the palaeographic determination of the age of the manuscripts. The use of carbon ink throughout the scrolls is also consistent with the known scribal practices of that time. There are, however, manuscripts, and among them the famous Genesis Apocryphon Scroll, which exhibit ink corrosion, normally associated with iron-gall inks.
Today, 60 years after their discovery, a community of scientists from the Jewish National and University Library (JNUL), the Technical University of Berlin (TU Berlin), the Federal Institute for Materials Research and Testing (BAM) and Fritz-Haber-Institute of the MPG (FHI) set out to scientifically investigate the finds of Qumran using the most modern methods. The results of the study will be used to determine the provenance of the texts as well as to contribute to their long-term preservation. A considerable part of the non-destructive investigation is taking place in the Berlin State Library and at the Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung , BESSY II.
Preliminary investigations, performed at the BAM on some fragments, were used to evaluate the extent to which X-ray analytical methods can provide information regarding the geographical origin of the fragments and match the individual pieces. The interpretation of the measurement results is made more difficult by age and storage of the objects. It is believed that ageing processes as well as conservation methods have altered the samples in addition to the changes caused by environmental influences.
In collaboration with the TU Berlin, the samples from the parchments found in the caves near Qumran were tested by means of three-dimensional synchrotron based X-ray fluorescence analysis (3D-SyXRF). The aim of this non-destructive investigation was the identification of the inorganic material used in the manufacture of the parchments.
The XRF experiments are supported by the non-destructive analysis by means of synchrotron based infrared spectroscopy (SyFTIR) in collaboration with BESSY II as well as optical and electron microscopy in collaboration with Fritz-Haber-Institute (FHI).
Material study of inks
(2016)
Our experimental knowledge about the inks of antiquity and late antiquity rarely goes beyond their visual description. In rare cases, inks typology has been determined by means of microscopy and reflectography, i.e. using their physical and optical properties, respectively. Soot, plant, and iron gall inks form different typological classes of historical black writing materials. Soot ink is a fine dispersion of carbon pigments in a water-soluble binding agent; plant-based ink consists of tannin solution; iron gall-ink presents a boundary case between soot and plant ink— a water soluble preliminary stage (similar to inks from the second group) oxidizes and evolves into a black, insoluble material (similar to the carbon pigments of the first group) when the writing is exposed to air. Each ink class has distinct properties that would readily permit their easy differentiation, if only these historical inks always belonged to just one of the classes above. In reality, inks may contain additives that obscure a clear picture.
Even crude observations suggest that the inks of antiquity differed greatly in their composition. We believe, that reconstructing the ink recipes with the help of advanced non-destructive analytical techniques could serve as a powerful accessory in the studies of ancient papyri.
The proposed paper will present a short survey of the methods of material analysis and the challenges offered by ancient inks. (Two) examples of ink studies from the collections of the Israel Museum in Jerusalem and Egyptian Museum in Berlin will conclude the paper.
The lecture will discuss the sensitive issue of authentication of the objects of cultural heritage of immense cultural and monetary value if certified to be genuine. It will be made clear that material analysis alone, especially its non-destructive variety conducted by specialists in a single technique, can not prove that the object is genuine. The best material analysis can do, after all appropriate tests have been conducted, is to announce that nothing has been found that contradicts the assumption of genuineness. Moreover, the results of the natural analysis can never be used as the only justification of the authentication in the cases of composite objects such as manuscripts or epigraphs. A certification always requires the expertise of the specialist in the field (be it a historian, paleographer, epigrapher, etc.), whose judgment can be at the most supported by appropriate material analysis.
The most effective approach for testing suspicious artifacts has been established by the forensic science. Here, not the authentication, but the determination of the forgery stands in the focus of the work. Investigation protocols developed within 150 years and constantly improved include a clear statement of the analysis purpose and the definition of plausibility criteria for the possible outcome. The younger sister of the forensics, archaeometry has to overcome additional obstacles such as the heterogeneity of historic material coupled with the scarcity of suitable reference material. Over the last two decades the popularity of archaeometric studies has increased enormously, with the industry-driven development of so-called non-destructive technologies (NDT) that do not require sampling. Further technological developments led to the appearance of NDT methods with extremely small interaction windows (µm range). Each of these methods has limitations that have to be carefully considered when planning the tests of a heterogeneous and often partially degraded historical material. This approach is inherently multi-instrumental, therefore archaeometric and forensic departments unite a number of specialists who work together defining the tasks and the methods involved for their successful completion.
The International Qumran project conducted at the BAM Federal Institute for Materials Research and Testing in 2007–10 aimed at establishing an optimal methodology for an accurate characterization of the Dead Sea Scrolls to address such questions as archaeological provenance, origin, and attribution of fragments to a specific sheet (Rabin 2013). Using equipment of various degrees of complexity we have shown that part of the historic information stored in the material can be revealed by proper characterization of the material. The on-site investigation of the Dead Sea Scrolls fragments from The Schøyen Collection in October 2012 offered the first chance to test this methodology in a field study. For the first time, we used mobile and non-invasive technology exclusively, since we could not transport all of our laboratory equipment to Norway for this project. Moreover, besides the technical limitations dictated by the available equipment, we had to cope with limited time: it was impossible to perform the number of scans required for optimal characterization of over 30 fragments within the fourteen days available. Nevertheless this study presents an important step in the material analysis of the Dead Sea Scrolls, since the devices we used are easily transportable, well known, and easily accessible throughout the world.
We have obtained a minute amount of dry ink scratched from the bronze inkwell MS 1655/2. The powder was stored between two glass slides to minimize contamination. For micro analysis by FTIR a sample of the ink powder was transferred into a diamond cell while for confocal Raman spectroscopy a micro sample was placed onto sticky tape. The same portion of the sample was also investigated by scanning electron microscopy, where the elements distribution was determined by EDX.
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.
The international Qumran project coordinated at the BAM, Berlin, resulted in an integrated methodology for determining the original and acquired properties of the skin-based writing surfaces of the Dead Sea Scrolls. This methodology offers a powerful tool for addressing such questions as the provenance, sorting and comparison of manuscripts. In addition, we have developed specific protocols for on-site studies, which were successfully applied to the fragments from the Schøyen collection in Norway. Our studies show that the Dead Sea Scrolls writing surfaces 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 first pilot study of the Geniza fragments, in which Babylonian and Palestinian traditions seem to follow the “eastern” and “western” technologies, respectively.
The evolution and socio-geographic distribution of writing inks in late Antiquity and the early Middle Ages build the second focus of the BAM group. We use X-ray fluorescence analysis (XRF) to determine the chemical composition of the inks and NIR-reflectography for their typology. Here the early appearance of the metal containing inks clearly belongs to the western tradition as opposed to the continuous use of soot inks in the East.
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.
Abstract For many years after the discovery of the Dead Sea Scrolls, text analysis and fragment attribution were the main concern of the scholars dealing with them. The uncertain archaeological provenance of a large part of the collection added an additional difficulty to the formidable task of sorting thousands of fragments. After sixty years of scholarly research, the questions of origin, archaeological provenance, and correct attribution of the fragments are still debated. In many cases, material characterization of the scroll writing media delivers answers to these questions. Physical and chemical examination of the skin-based material of the Dead Sea Scrolls started shortly after their discovery. Subsequent studies dedicated to long-term preservation resulted in a respectable body of knowledge about this material, in many ways very different from medieval parchment. A new multi-instrumental approach, developed for an accurate characterization of the highly inhomogeneous 'parchment' of the Dead Sea Scrolls, might lead to a reliable reconstruction of their history. This approach is illustrated by the case studies, in which we discuss the specific questions of origin (1QHa), archaeological provenance (11QTa), and post-discovery interventions (1QapGen ar).
It is well documented that throughout Antiquity, ancient Egyptians used mostly carbon inks as a writing material. In Late Antiquity, some metals started to be added to carbon based inks. We have records of five manuscripts from the Dead Sea Scrolls collection whose carbon inks were found to contain copper Also, lead was recently found as an additive in carbon inks on a charred fragment from Herculaneum. Furthermore, the earliest evidence of iron-gall ink was found in the Book of Proverbs (Codex Ms. Berol. orient. oct. 987) dating to the third fourth centuries ce. It has been suggested that along with carbon and iron-gall inks, there is no reason to think that purely tannin inks were not also in use in Egypt. However, so far, we just have evidence of a copper-tannin ink identified in a number of documents from Egypt in the first third centuries bce. In an attempt to fill this gap in this extremely fragmented scenario during our studies of the socio-geographic history of inks, we arrived at the conclusion that the continuous production of Coptic manuscripts from Late Antiquity to the Middle Ages offers a unique opportunity for the historical study of inks across a large geographic area.
Advanced codicological studies of Cod. germ. 6 (Hamburg, Staats- und Universitätsbibliothek): Part 2
(2018)
The work presented here follows the article Combining Codicology and X-Ray Spectrometry to Unveil the History of Production of Codex germanicus 6 (Staats- und Universitätsbibliothek Hamburg), published in 2014.1 It confirms the main result of the previous article: the Artusnotiz, the fourth text in the bound manuscript, must have been introduced as the last one. This paper offers further details of the codex production, based on the composition of the black and red inks collected in four measurement campaigns. Furthermore, using imaging μ-XRF, we succeeded in understanding the strong variation of the composition of the red inks in the initials of all the texts except for Parzival and Jeanne d’Arc.
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).
A combination of 3D micro X-ray fluorescence spectroscopy (3D micro-XRF) and micro-XRF was utilized for the investigation of a small collection of highly heterogeneous, partly degraded Dead Sea Scroll parchment samples from known excavation sites. The quantitative combination of the two techniques proves to be suitable for the identification of reliable marker elements which may be used for classification and provenance studies. With 3D micro-XRF, the three-dimensional nature, i.e. the depth-resolved elemental composition as well as density variations, of the samples was investigated and bromine could be identified as a suitable marker element. It is shown through a comparison of quantitative and semiquantitative values for the bromine content derived using both techniques that, for elements which are homogeneously distributed in the sample matrix, quantification with micro-XRF using a one-layer model is feasible. Thus, the possibility for routine provenance studies using portable micro-XRF instrumentation on a vast amount of samples, even on site, is obtained through this work.