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Medieval Pb (Cu-Ag) Smelting in the Colline Metallifere District (Tuscany, Italy): Slag Heterogeneity As a Tracer of Ore Provenance and Technological Process

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Medieval Pb (Cu-Ag) Smelting in the Colline Metallifere District (Tuscany, Italy): Slag Heterogeneity As a Tracer of Ore Provenance and Technological Process minerals Article Medieval Pb (Cu-Ag) Smelting in the Colline Metallifere District (Tuscany, Italy): Slag Heterogeneity as a Tracer of Ore Provenance and Technological Process Laura Chiarantini 1,* , Marco Benvenuti 2 , Giovanna Bianchi 3, Luisa Dallai 3, Vanessa Volpi 3,4 and Rosarosa Manca 2 1 Centro di Microscopia Elettronica e Microanalisi, Università di Firenze, Via. G. Capponi 3r, 50121 Florence, Italy 2 Dipartimento di Scienze della Terra, Università di Firenze, Via G. La Pira 4, 50121 Firenze, Italy; m.benvenuti@unifi.it (M.B.); rosarosa.manca@unifi.it (R.M.) 3 Dipartimento di Scienze Storiche e dei Beni Culturali, Università di Siena, Via Roma 56, 53100 Siena, Italy; [email protected] (G.B.); [email protected] (L.D.); [email protected] (V.V.) 4 Dipartimento di Biotecnologie, Chimica e Farmacia, Università di Siena, Via A. Moro 2, 53100 Siena, Italy * Correspondence: laura.chiarantini@unifi.it; Tel.: +39-055-2757792 Abstract: Archaeological investigations of the Colline Metallifere district (Southern Tuscany, Italy) have highlighted several Medieval sites located close to the main Cu-Pb-Fe (Ag) ore occurrences. This study is focused on the investigation of late-medieval slags from Cugnano and Montieri sites using both geochemical and mineralogical methods to understand slag heterogeneities as result of ore differences and technological processes. Matte-rich slags present in both sites (with abundant matte ± speiss and frequent relict phases) represent waste products related to primary sulphide ore smelting to obtain a raw lead bullion. The distribution of slags between the Ca-rich or Fe-rich dominant composition, and the consequent mineralogy, are tracers of the different ore–gangue Citation: Chiarantini, L.; Benvenuti, M.; Bianchi, G.; Dallai, L.; Volpi, V.; association that occurred in the two sites. Silver is present only in very small matte-rich slags and Manca, R. Medieval Pb (Cu-Ag) ores enclosed within the mortar of the Montieri site; wastes derived from silver-rich mineral charges Smelting in the Colline Metallifere were probably crushed for the recovery of silver. Matte-poor slags found at Montieri represent a District (Tuscany, Italy): Slag second smelting; raw lead bullion obtained from matte slags (both Fe- and Ca-rich) was probably Heterogeneity as a Tracer of Ore re-smelted, adding silica and Al2O3-phase-rich fluxes, under more oxidizing conditions to reduce Provenance and Technological metal impurities. This second step was probably employed for Zn-rich lead ores; this process helped Process. Minerals 2021, 11, 97. to segregate zinc within slags and improve the quality of the metal. https://doi.org/10.3390/min11020097 Keywords: slags; archaeometry; archaeology; medieval; lead; zinc; silver; smelting; Tuscany Received: 15 December 2020 Accepted: 14 January 2021 Published: 20 January 2021 1. Introduction Publisher’s Note: MDPI stays neutral with regard to jurisdictional claims in The Colline Metallifere district (near Massa Marittima, southern Tuscany) hosts many published maps and institutional affil- Cu-Pb-Zn (Ag) vein deposits, which fed an important mining and metallurgical industry iations. from the Chalcolithic period up to the 1970s. According to archaeological and historical documents, during the medieval period (12th–14th century AD), the metal production of this area was mainly focused on the extraction of copper and silver for coinage. Archaeological campaigns of the renowned castle of Rocca San Silvestro [1,2] high- lighted the presence of mining sites intrinsically connected to the process of castle formation. Copyright: © 2021 by the authors. Licensee MDPI, Basel, Switzerland. This aspect suggests that during the development of local seigneurships, in this geographi- This article is an open access article cal context, much of their economic power was based on controlling and exploiting metals. distributed under the terms and The Colline Metallifere project, which began in the mid-1980s, aimed to study the rela- conditions of the Creative Commons tionships between the location of medieval settlements and mineral resources. Particular Attribution (CC BY) license (https:// interest was focused on how local communities controlled and organized metallurgical creativecommons.org/licenses/by/ production during the medieval period [3]. After the castle of Rocca San Silvestro, extensive 4.0/). research was performed on other sites with specific mining vocation, such as Campiglia Minerals 2021, 11, 97. https://doi.org/10.3390/min11020097 https://www.mdpi.com/journal/minerals Minerals 2021, 11, x FOR PEER REVIEW 2 of 21 The Colline Metallifere project, which began in the mid-1980s, aimed to study the relationships between the location of medieval settlements and mineral resources. Partic- Minerals 2021, 11, 97 ular interest was focused on how local communities controlled and organized metallurgi-2 of 23 cal production during the medieval period [3]. After the castle of Rocca San Silvestro, ex- tensive research was performed on other sites with specific mining vocation, such as Cam- Marittima,piglia Marittima, Suvereto, Suvereto, Donoratico, Donoratico, Rocchette Rocchette Pannocchieschi, Pannocchieschi, Montemassi, Montemassi, Cugnano, Cugnano, and Roccaand Rocca degli degli Alberti Alberti at Monterotondo at Monterotondo Marittimo Marittimo [4–7]. The[4–7]. project The project continued continued in recent in yearsrecent withyears the with excavations the excavations at the siteat the of Cugnano,site of Cugnano, with a with large-scale a large project-scale project in the municipalityin the munic- ofipality Montieri of Montieri (including (including excavations excavations and field and surveys), field surveys), and with and the with investigations the investigations at the alumat the mines alum sitemines of Monteleosite of Monteleo [8–10]. [8–10]. ThisThis studystudy is focused on on the the analysis analysis of of slag slag recovered recovered from from the the sites sites of Cugnano of Cugnano and andMontieri. Montieri. Several Several heaps heaps of metallurgical of metallurgical slags slags that dated that dated to a wide to a widehistorical historical period period (11th– (11th–14th14th centuries) centuries) were werediscovered discovered during during archaeological archaeological excavations. excavations. The Theslags slags were were ana- analyzedlyzed using using optical optical microscopy, microscopy, SEM SEM-EDS,-EDS, XRD, XRD, ICP ICP-OES,-OES, ICP ICP-MS-MS and and INAA INAA with with the theaim aim of characterizing of characterizing the thearchaeometallurgical archaeometallurgical activity activity performed performed in these in these sites. sites. The Thedata dataprovide provide us with us with an extremely an extremely complex complex picture picture of the of different the different metallurgical metallurgical activities activities car- carriedried out out in inthis this area area,, with with many many aspects aspects still still to tobe be clarified clarified.. 2.2. GeologyGeology andand OreOre MineralogyMineralogy TheThe Southern Southern Tuscany Tuscany area area is locatedis located in ain portion a portion of the of Northernthe Northern Apennines Apennines orogenic oro- belt,genic which belt, iswhich a Tertiary is a Tertiary thrust and thrust fold beltand vergingfold belt to verging NE-SW andto NE resulting-SW and from resulting the closure from ofthe the closure Ligurian-Piedmont of the Ligurian Ocean-Piedmont and the Ocean subsequent and the collision subsequent between collision the Adria between micro- the plateAdria and micro the- Europeanplate and the Plate. European Within thePlate. tectonic Within pile, the the tectonic lower pile units, the were lower deposited units were on thedeposited continental on the Adria continental Plate (the Adria continental Plate Tuscan(the continental Domain and Tuscan epi-continental Domain and Subligurian epi-conti- Domain).nental Subligurian The top units—known Domain). The as thetop Ligurianunits—known Domain—represent as the Ligurian sediments Domain and—represent portion ofsediments oceanic crust and portion (Figure1 of). oceanic crust (Figure 1). FigureFigure 1.1. Schematic geologic geologic map map of of southern southern Tuscany Tuscany with with location locationss of ofthe the main main ore oredeposits. deposits. (1) Acid igneous or subvolcanic rocks, dykes and sills, volcanic rocks, and pyroclastic deposits; (2) (1) Acid igneous or subvolcanic rocks, dykes and sills, volcanic rocks, and pyroclastic deposits; conglomerates, sandstones, clays, evaporites, and sands; (3) limestones, marl, sandstones, and (2) conglomerates, sandstones, clays, evaporites, and sands; (3) limestones, marl, sandstones, and mudstones (late Cretaceous–Early Paleocene), shales, siltstones, and limestones (early Cretaceous), mudstones (late Cretaceous–Early Paleocene), shales, siltstones, and limestones (early Cretaceous), ophiolites (Jurassic); (4) sandstones, conglomerates, shales, limestones, and siltstones (Paleocene– Miocene); (5) from bottom: limestone formations, radiolarites, shales, marls, calcilutites, calcarenites, and sandstone flysh (late Triassic–early Miocene). Minerals 2021, 11, 97 3 of 23 Metal deposits in the Colline Metallifere district are mostly characterized by Cu-Pb-Zn (Ag) vein bodies associated with late-Apenninic tectonic lineaments and emplaced by magmatic-meteoric hydrothermal fluids in the late stage of the Apenninic orogeny [11]. The more significant silver-rich mineralizations are located between Montieri and Massa
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