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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.
Parchment has been in use for thousands of years
and has been used as the writing or drawing support for
many important historic works. A variety of analytical
techniques is currently used for routine assessment of the
degree of denaturation of historic parchment; however,
because parchment has a heterogeneous nature, analytical
methods with high spatial resolution are desirable. In this
work, the use of small-angle X-ray scattering (SAXS) and
synchrotron-IR (SR-IR) was examined in conjunction with
multivariate data analysis to study degradation of an
extended set of historic parchment samples, and particularly
to investigate the effect of lipids and the presence of iron
gall ink on the degradation processes. In the data analysis,
shrinkage temperature, lipid content, sample age, presence
of ink and accelerated degradation were included. The
analysis of loading factors in partial least-squares regression
and principal component analyses based on SAXS, SR-IR
and other analytical and descriptive data reveals the effect
of lipid removal on diffraction patterns, and lipids are found
to cause the degradation process in parchment to accelerate.
The effect of iron gall ink is also evident, although the
mechanism of ageing is different to that of natural ageing in
the absence of ink. In addition, a historic parchment score
from ca. 1750 is examined, demonstrating the significant
effect of iron gall ink, and lipids and inorganic soiling on its
increased degradation.
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).
The library of the remote monastery of Qäqäma Maryam Kidanä Mehrät in Däg'a Tämben (Tagray, North Ethiopia) was investigated by the team of the project Ethio-SPaRe in June and November 2012. A preliminary study of the library showed that the collection was extended and profoundly renovated in the nineteenth Century, in the course of the revival the monastery had during the reign of King Yohannas IV (1872-89). The shaping of the collection was apparently linked to the figure of the powerful abbot, Gäbrä Giyorgis, who donated dozens of books of diverse provenance, which he himself gathered or received as gifts.1 As the result, the extensive library contains a huge amount of information, but its heterogeneity poses a very serious challenge to the researcher.
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.