The contribution of geochemical and mineralogical characterization of iron slags in provenance studies in the Podravina region, NE Croatia
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Jan 20, 2022
Keywords:
iron production, XRD, ICP-MS/AES, trace elements, NRC ratios, PCA, bog iron ore
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Abstract
Archaeological excavations in the Podravina region led to discovery of sites with traces of bloomery iron production during Late Antiquity and the Early Middle Ages. Mineralogical analysis of the slags recognized fayalite as the main mineral phase, while geochemical analysis confirmed high Fe contents, typical for bloomery iron smelting. Based on the previously established occurrences of bog iron ores in the study area, provenance studies were carried out using trace and rare earth elements to create a geochemical signature. Similar shapes and patterns of bog iron ores and iron slag signatures imply a genetic connection between the ore and the slag, as well as variation related to the temporal and spatial context of both slags and ores.
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References
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BOTIĆ, K. (2021): Absolute dating of Virje and Hlebine sites.− In: SEKELJ IVANČAN, T. & KARAVIDOVIĆ, T. (eds.): Interdisciplinary Research into Iron Metallurgy along the Drava River in Croatia - The TransFER Project, Oxford: Archaeopress, 92–100. doi: 10.32028/9781803271026-5
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BRENKO, T., BOROJEVIĆ ŠOŠTARIĆ, S., RUŽIČIĆ, S. & SEKELJ IVANČAN, T. (2020): Evidence for the formation of bog iron ores in the soils of the Podravina region, NE Croatia: Geochemical and mineralogical study.− Quatern. Int., 536, 13–29. doi: 10.1016/j.quaint.2019.11.033
BRKIĆ, Ž. & BRIŠKI, M. (2018): Hydrogeology of the western part of the Drava Basin in Croatia.− J. Maps., 14, 173–177. doi: 10.1080/17445647.2018.1445043
BRKIĆ, Ž., LARVA, O. & URUMOVIĆ, K. (2010): The quantitative status of the groundwater in alluvial aquifers in northern Croatia.− Geol. Croat., 63, 283–298. doi: 10.4154/GC.2010.23
CHARLTON, M.F., CREW, P., REHREN, TH. & SHENNAN, S.J. (2010): Explaining the evolution of ironmaking recipes–an example from northwest Wales.− J. Anthropol. Archaeol., 29, 352–367. doi: 10.1016/j.jaa.2010.05.001
CHARLTON, M.F., BLAKELOCK, E., MARTINÓN-TORRES, M. & YOUNG, T. (2012): Investigating the production provenance of iron artifacts with multivariate methods.− J. Archaeol. Sci., 39, 2280–2293. doi: 10.1016/j.jas.2012.02.037
COUSTURES, M.P., BÉZIAT, D. & TOLLON, F. (2003): The use of trace element analysis of entrapped slag inclusions to establish ore – bar iron links: examples from two Gallo-roman iron-making sites in France (Les Martys, Montagne Noire, and Les Ferrys, Loiret).− Archaeometry, 45, 599–613. doi: 10.1046/j.1475-4754.2003.00131.x
CREW, P. (2000): The influence of clay and charcoal ash on bloomery slags.− In TIZZONI, C.C. & TIZZONI M. (eds.): Iron in the Alps: Deposits, Mines and Metallurgy from Antiquity to the XVI Century, Bienno, p. 38–48.
DESAULTY, A-M., DILLMANN, P., L’HÉRITIERA, M., MARIET, C., GRATUZE, B., JORON, J-L. & FLUZIN, P. (2009): Does it come from the Pays de Bray? Examination of an origin hypothesis for the ferrous reinforcements used in French medieval churches using major and trace element analyses.− J. Archaeol. Sci., 36, 2445–2462. doi: 10.1016/j.jas.2009.07.002
DEVOS, W., SENN-LUDER, M., MOOR, C. & SALTER, C. (2000): Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) for spatially resolved trace analysis of early-medieval archaeological iron finds.− Int. J. Anal. Chem., 366, 873–880. doi: 10.1007/s002160051588
DILLMANN, P. & L’HÉRITIER, M. (2007): Slag inclusion analyses for studying ferrous alloys employed in French medieval buildings: supply of materials and diffusion of smelting processes.– J. Archaeol. Sci, 34/11, 1810–1823. doi: 10.1016/j.jas.2006.12.022
FULLER, A.J., SHAW, S., WARD, M.B., HAIGH, S.J., MOSSELMANS, F.W., PEACOCK, C.L. STACKHOUSE, S., DENT, A.J., TRIVEDI, D. & BURKE, I.T. (2015): Caesium incorporation and retention in illite interlayers.– Appl. Clay Sci., 108, 128–134. doi: 10.1016/j.clay.2015.02.008
GINGELE, F.X. & DE DECKKER, P. (2005): Clay mineral, geochemical and Sr-Nd isotopic fingerprinting of sediments in the Murray-Darling fluvial system, southeast Australia.– Aust. J. Earth Scie., 52, 965–974. doi: 10.1080/08120090500302301
GORDON, R.B. (1997): Process deduced from ironmaking wastes and artefacts.− J. Archaeol. Sci., 24, 9–18. doi: 10.1006/jasc.1995.0092
HEAD J. M. (2019). Formal subdivision of the Quaternary System/Period: Present statu and future directions.− Quatern. Int., 500, 32–51. doi: 10.1016/j.quaint.2019.05.018
HEIMANN, R.B., KREHER, U., SPAZIER, I. & WETZEL G. (2001): Mineralogical and chemical investigations of bloomery slags from prehistoric (8th century BC to 4th century AD) iron production sites in Upper and Lower Lusatia, Germany.− Archaeometry, 43, 227–252. doi: 10.1111/1475-4754.00016
HELLEBRANDT, S.E., HOFMANN, S., JORDAN, N., BARKLEIT, A. & SCHMIDT, M. (2017): Incorporation of Eu(III) into Calcite under Recrystallization conditions.− Sci. Rep-UK., 6, 33137. doi: 10.1038/srep33137
HORST-MADSEN, L. & BUCHWALD, V.F. (1999): The characterisation and provenancing of ore, slag and iron from the Iron Age settlement in Snorup.− The Journal of the Historical Metallurgy Society, 33/2, 57–67.
KACZOREK, D. & SOMMER, M. (2003): Micromorphology, chemistry and mineralogy of bog iron ores from Poland.− Catena, 54, 393–402. doi: 10.1016/S0341-8162(03)00133-4
KĄDZIOŁKA, K., PIETRANIK, A., KIERCZAK, J., POTYSZ, A. & STOLARCZYK, T. (2020): Towards better reconstruction of smelting temperatures: Methodological review and the case of historical K-rich Cu-slags from the Old Copper Basin, Poland.− J. Archaeol. Sci., 118, 105142. doi: 10.1016/j.jas.2020.105142
KARAVIDOVIĆ, T. (2020): Rekonstrukcija postupka prženja rude: eksperimentalni pristup.− In: VITEZOVIĆ, S., ANTONOVIĆ, D. & ŠARIĆ, K. (eds.):Aktuelna interdisciplinarna istraživanja tehnologije u arheologiji Jugoistočne Europe, Zbornik radova prvog skupa sekcije za arheometriju, arheotehnologiju i eksperimentalnu arheologiju Srpskog arheološkog društva, [Current interdisciplinary technology in archaeology research of south-eastern Europe, Proceedings from first meeting of archaeometry, archaeotechnology and experimental archaeology of Serbian Archaeological Society], 130–137.
KONGOLI, F. & YAZAWA, A. (2001): Liquidus surface of FeO-Fe2O3-SiO2-CaO slag containing Al2O3, MgO, and Cu2O at intermediate oxygen partial pressures.− Metall. Mater. Trans. B., 32, 583–592. doi: 10.1007/s11663-001-0114-7
KOPIĆ, J., LOBOREC, J. & NAKIĆ, Z. (2016): Hydrogeological and hydrogeochemical characteristics of a wider are of the regional well field Eastern Slavonia – Sikirevci.− The Mining-Geological-Petroleum Bulletin, 31, 47–66. doi: 10.17794/rgn.2016.3.4
LANDUYDT, C.J. (1990): Micromorphology of iron minerals from bog ores of the Belgian Campine area.− Dev. Soil Sci., 19, 289–294. doi: 10.1016/S0166-2481(08)70340-4
LINTJEWAS, L. & SETIAWAN, I. (2018): Mobility of rare earth element in hydrothermal process and weathering product: a review.− IOP Conf. Series: Earth and Environmental Science, 118. doi: 10.1088/1755-1315/118/1/012076
LÓCZY, D., DEZSŐ, J., CZIGÁNY, S., GYENIZSE, P., PIRKHOFFER, E. & HALÁSZ, A. (2014): Rehabilitation potential of the Drava River floodplain in Hungary.− In: 2nd International Water Resources and Wetlands. Conference Paper.
MANASSE, A. & MELLINI, M. (2002): Chemical and textural characterization of medieval slags from the Massa Marittima smelting sites (Tuscany, Italy).− J. Cult. Herit., 3, 187–198. doi: 10.1016/S1296-2074(02)01176-7
MAES, E., ISERENTANT, A., HERBAUTS, J. & DELVAUX, B. (1999): Influence of the nature of clay minerals on the fixation of radiocaesium traces in an acid brown earth-podzol weathering sequence.− Eur. J. Soil Sci., 50, 117–125. doi: 10.1046/j.1365-2389.1999.00224.x
MORTON, G. R., & WINGROVE, J. (1969): Constitution of bloomery slags, part 1: Roman.− J. Iron Steel I., 207, 1556–1564.
NAVASAITIS, J. & SELSKIENĖ, A. (2007): Metallographic Examination of Cast Iron Lump Produced in the Bloomery Iron Making Process.− Mat. Sci., 13/2, 167–173.
NAVASAITIS, J., SELSKIENĖ, A. & ŽALDARYS, G. (2010): The Study of Trace Elements in Bloomery Iron.− Mater. Sci.+, 16/2, 113–118.
NEMET, I., RONČEVIĆ, S., BUGAR, A., ZUBIN FERRI, T. & PITAREVIĆ, L. (2018): Classification analysis of archaeological findings from early-iron production (Turopolje region, NW Croatia) based on multi-analytical profiling.− J. Anal. Atom. Spectrom., 33, 2053–2061. doi: 10.1039/C8JA00202A
PLEINER, R. (1967): Die Technologie des Schmiedes in der Großmährischen Kultur.− Slovenská Archeológia, 15/1, 77–188.
PLEINER, R. (2000): Iron in Archaeology. The European Bloomery Smelters.− Archeologický ústav AV CR, Prague, 400 p.
POLLARD, M. & HERON, C. (1996): Archaeological Chemistry.− Royal Society of Chemistry, Cambridge, 456 p. doi: 10.1039/9781847550156
PORTILLO-BLANCO, H., CRUZ ZULUAGA, M., ANGEL ORTEGA, L., ALONSOOLAZABAL, A., CEPEDA-OCAMPO, J.J. & MARTINEZ SALCEDO, A. (2020): Mineralogical Characterization of Slags from the Oiola Site (Biscay, Spain) to Assess the Development in Bloomery Iron Smelting Technology from the Roman Period to the Middle Ages.− Minerals-Basel, 10, 321. doi: 10.3390/min10040321
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