Mössbauer spectrometry applied to the study of laboratory samples made of iron gall ink

Iron gall inks consist of a mixture of vitriol, gall nut extracts and gum arabic. The association of the iron(II) sulphate present in vitriols, and the carboxyphenolic acids present in gall nut extracts leads to the formation of dark coloured iron-based precipitates. In order to evaluate the percentage of iron used in the formation of these precipitates, transmission Mössbauer spectroscopy (MS) measurements were performed on laboratory made inks at room temperature. These were completed by X-ray diffraction (XRD), and Raman spectroscopy measurements. The samples consisted of several solutions of iron(II) sulphate, gallic acid and gum arabic. After evaporation, the residues were analysed. Up to eight different Mössbauer signatures were detected, most of them correlated to iron sulphates. The Mössbauer signature of the iron gall precipitate was also isolated. It is not distinctly defined and may overlap with the signatures of iron(III) hydroxy-sulphates, such as jarosite or copiapite. Raman spectrometry then proved to be a useful complementary technique for the identification of the precipitate

Ancient inks: a forensic art historical perspective

N