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Fe K-edge X-ray absorption near edge structure (XANES) and Mossbauer spectra were collected on synthetic glasses of basaltic composition and of glasses on the sodium oxide-silica binary to establish a relation between the pre- edge of the XANES at the K-edge and the Fe oxidation state of depolymerised glasses. Charges of sample material were equilibrated at ambient pressure, superliquidus temperatures and oxygen fugacities that were varied over a range of about 15 orders of magnitude. Most experiments were carried out in gas-flow furnaces, either with pure oxygen, air, or different CO/CO2 mixtures. For the most reduced conditions, the samples charges were enclosed together with a pellet of the IQF oxygen buffer in an evacuated silica glass ampoule. Fe3+/SigmaFe x 100 of the samples determined by Mossbauer spectroscopy range between 0% and 100%. Position and intensity of the pre-edge centroid position vary strongly depending on the Fe oxidation state. The pre-edge centroid position and the Fe oxidation state determined by Mossbauer spectroscopy are nonlinearly related and have been fitted by a quadratic polynomial. Alternatively, the ratio of intensities measured at positions sensitive to Fe2+ and Fe3+, respectively, provides an even more sensitive method. Pre- edge intensities of the sample suite indicate average Fe co-ordination between 4 and 6 for all samples regardless of oxidation state. A potential application of the calibration given here opens the possibility of determining Fe oxidation state in glasses of similar compositions with high spatial resolution by use of a Micro-XANES setup (e.g., glass inclusions in natural minerals). (C) 2004 Elsevier B.V. All rights reserved
We studied the oxidation and migration processes of inorganic compounds in iron gall inks with a combination of micro X-ray fluorescence analysis (micro-XRF) and micro X-ray absorption near edge structure spectroscopy (micro-XANES). With elemental mapping by micro-XRF, the correlation of the minor elements in the ink to the major element Fe was investigated. Along concentration profiles of Fe, micro-XANES measurements were carried out in order to determine the oxidation state and the local environment. With the help of model inks, we could show that Cu is a further important element in the paper degradation process due to iron gall ink corrosion. (C) 2004 Elsevier B.V. All rights reserved