TY - CONF A1 - Schmid, Thomas A1 - Dariz, P. ED - Ziemann, M. T1 - Raman band widths of anhydrite II reveal the burning history of high-fired medieval gypsum mortars T2 - Book of abstracts and conference programme: 10th international congress on the application of Raman spectroscopy in art and archaeology N2 - The use of high-fired gypsum as binder for masonry and joint mortars or stuccowork in Central Europe in the Early and High Middle Ages was a regional specific as it depended on local gypsum deposits. The calcination technology possible at the time resulted in an assemblage of calcium sulphate phases dehydrated to different degrees and partly thermally damaged accessory minerals of the raw gypsum. Because of the absence of medieval textbooks, the observation of high-temperature, low-pressure mineral transformations and the correlation of phases coexisting in not hydrated binder relicts in the gypsum matrix to the mineralogy of the raw material and the burning conditions constitute the only source to the historical technological know-how. The CaSO4–H2O system consists of five crystalline phases, which can be discriminated by structural analysis methods, such as Raman spectroscopy, due to obvious differences in their spectroscopic data: gypsum (CaSO4 ⋅ 2 H2O), bassanite (hemihydrate, CaSO4 ⋅ ½ H2O), anhydrite III (CaSO4), anhydrite II (CaSO4), and anhydrite I (CaSO4). Only recently, it was possible to demonstrate that small spectroscopic variations exist also within the relatively large stability range of anhydrite II from approx. 180°C to 1180°C: all Raman bands narrow with increasing burning temperature applied in the synthesis from gypsum powder. The determination of band widths of down to 3 cm-1 and differences between them of a few tenths of a wavenumber is not a trivial task. Thus, this contribution discusses peak fitting and strategies for correction of instrument-dependent band broadening. Raman maps of polished thin sections of gypsum mortars provide access to the burning histories of individual remnant thermal anhydrite grains and enable the discrimination of natural anhydrite originating from the gypsum deposit. This novel analytical method was applied to samples from medieval South Tyrolean stucco decorations and sculptures. Beyond that, Raman microspectroscopy was employed for following pyrometamorphic reactions in natural impurities of the raw material. In the presented examples mineral thermometry indicates process temperatures above 800°C: the breakdown of magnesium-rich chlorite led to the formation of forsterite Mg2SiO4, while the thermal decomposition of dolomite CaMg(CO3)2 yielded – after hydration and carbonation – magnesite MgCO3, CaCO3 polymorphs and magnesian calcite. Lower burning temperatures, which leave the accessory minerals in their pristine form, can be traced by measuring the spectra of anhydrite crystalites in grains of firing products and evaluating Raman band widths. Throughout the applications of this analytical method so far, calcination temperatures ranging from approx. 600°C to 900°C were determined. T2 - 10th International Congress on the Application of Raman Spectroscopy in Art and Archaeology CY - Potsdam, Germany DA - 03.09.2019 KW - Raman microspectroscopy KW - High-fired medieval gypsum mortars KW - Raman band width KW - Gypsum dehydration KW - Thermal anhydrite PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-496204 SP - 36 EP - 37 PB - University of Potsdam CY - Potsdam AN - OPUS4-49620 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmid, Thomas A1 - Dariz, P. T1 - Research in the SALSA Application Lab – Shedding light onto high-fired medieval gypsum mortars N2 - After an introduction into the SALSA lab building and the ideas and sources of inspiration for building up the Application Lab as a spectroscopy lab with a strong focus on imaging and microspectroscopy, a very successful example of an interdisciplinary collaboration between the fields of art technology and analytical sciences is presented. T2 - Make and Measure 2019 CY - Berlin, Germany DA - 25.10.2019 KW - Interdisciplinary research KW - Teaching KW - High-fired medieval gypsum mortars KW - Raman spectroscopy PY - 2019 AN - OPUS4-49623 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmid, Thomas A1 - Dariz, P. T1 - Raman band widths of anhydrite II reveal the burning history of high‐fired medieval gypsum mortars N2 - An interdisciplinary collaboration between art technology and analytical sciences yielded an approach based on Raman microspectroscopy for the determination of the burning temperatures applied during the production process of high-fired medieval gypsum mortars. Analytical challenges and applications of the approach to examples from the cultural heritage of South Tyrol are presented. T2 - 10th International Congress on the Application of Raman Spectroscopy in Art and Archaeology CY - Potsdam, Germany DA - 03.09.2019 KW - Raman microspectroscopy KW - High-fired medieval gypsum mortars KW - Thermal anhydrite PY - 2019 AN - OPUS4-49624 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -