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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.
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.
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 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 collection Manuscripta Americana in Berlin consists of fragmented codices acquired by Alexander von Humboldt in Mexico. Some of these Humboldt Codices are published as hieroglyphic writings of the Aztecs in “Vues des Cordilleres et Monuments des Peuples indigènes de l’Amerique”. Starting from a special compilation of seven fragments on plate 36 in the “Atlas”, we investigated the corresponding original fragments using material analysis in order to clarify their historical relations. The analyses were carried out with X-ray fluorescence analysis, VIS spectroscopy, and infrared spectroscopy in diffuse reflection and revealed typical indigenous colors like cochineal, indigo, and organic yellows (e.g. mangrove and zacatlaxcalli). Four fragments under investigation show exactly the same material and thus must once have belonged together in one compendium. An additional manuscript from Mizquiahuala also shown on plate 36 can be matched to another one that is not published in the “Atlas”.
The presented Humboldt Codices are from the early colonial period of Mexico and originate from different localities
1. typical indigen colors and mixtures:
cochineal (red), indigo (blue and green), carbon (black),
mangle, zacatlaxcalli, organic (brown, yellow)- critical!
2. colonial influence:
iron gall ink for writing
3. single fragments belong together:
are cut (fragments IX-XII),
from Mizquahuala distributed (VII, XIII, XIV, [XV]) (VII, XIII in Mexico, XIV in Paris)
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 mayor part of the Berlin collection `Manuscripta Americana´ consists of documents compiled by Alexander von Humboldt. The diversity of the written fragments and their shape presume few accordance concerning purpose, place or time of production. Even before the papers came to Berlin, manuscripts were copied, divided and collected by famous scholars also in Mexico. Back in Europe, Humboldt visited further collections and published the detected hieroglyphic writings altogether with cultural objects and landscapes in the book `Vues des Cordillères et Monuments des Peuples Indigènes de l`Amerique, voyage de Humboldt et Bonpland´, labelled corresponding to the cultural background.
By scientific and culture historical analyses, the Humboldt codices are revised and related to each other and others. In especial, the compilation of fragments shown on plate 36 in the book is looked at more closely. Whereas most of the plates represent only one sheet of painted amate paper, here segments with details of seven fragments are put together. It is tried to comprehend why these pieces are on one plate.
To find out a common feature of the documents, their content and represented form are compared. A correlation between some pieces is obvious and thus is also expected in the manufacture of the codices, in the kind of material used. For this the inks and colors are determined by scientific analysis including XRF-, Raman-, FTIR- and VIS- spectroscopy. Special material is detected and related to results of former analysis of codices written during the colonial period of America. Herewith a clear cultural assignment of the manuscripts is performed.
A relation of the fragments represented on plate 36 among each other and to other codices of the collection Manuscripta Americana in Berlin is discussed. Also, if the manuscripts are unique `originals´ or represent fragments of documents, whose corresponding pieces maybe found- in the best case- incorporated in other collections. We detected, that at least two of them can be put into relation to similar manuscripts deposited in Mexico. Further material analysis should clarify, if the corresponding pieces are identical- from one document, or if one of them is a copy. Herewith an approximation to authenticity features and history is issued.
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.
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.
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.
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.
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.
X-ray fluorescence analysis, due to its non-destructive nature and ist suitability to work with historic objects in situ, quickly became one of the most important methods for the evaluation of iron-gall ink. The main advantage of this qualitative and semi-quantitative method is that it makes it easy to differentiate between inks, based on the assumption that the differences result from the manufacture of the ink.
This work explores the question whether the ink ‘fingerprint’ results strictly from the elemental composition of the basic ink ingredients even if it is stored in vessels made of metals or metal alloys. In addition, we tested and compared the performance of three different XRF spectrometers.
We prepared various lab-grade inks according to historical ink recipes and measured the metal content of the ink deposited on sized cotton Linters paper with three types of XRF spectrometers: a simple hand-held device with an interaction spot of 4 mm and two devices equipped with poly-capillary Xray optics for line scanning and imaging. Since the exact elemental mass composition of the non-aged ink samples was known, we were able to evaluate the accuracy of the research procedure. Lab-grade inks were then aged in the metal jars imitating inkwells. The aging of the inks in the metal containers resulted in the significant change of the primary inks fingerprint as opposed to that of the control inks stored in glass containers. This effect was independently confirmed by the measurements conducted with every instrument we used. We will present a brief comparison of the results 43 achieved when using different spectrometers and a possible hypothesis explaining the processes that occurred.
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 Weimar research project has set the goal of placing style-critical research on Old Master drawings on a new, methodologically proven foundation. The starting point is the stock of Dutch drawings possessed by the Klassik Stiftung Weimar, whose extent (ca. 1,400 items) and character make it one of the most significant outside the Netherlands. The focus here is on drawings that were executed with red chalk. This drawing material has different functions - one of which is the use as a transmission material. The methodological approach is double: first, the scientific indexing of this stock. The foundations for this, along with classic analysis of style, are innovative material-scientific methods of investigation.