Decoding bronze production at Terramara Santa Rosa di Poviglio site (Bronze Age, N Italy): Insights from secondary production waste

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Rademakers, Andrea Zerboni, and 1 more This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-6572450/v1 This work is licensed under a CC BY 4.0 License Status: Published Journal Publication published 05 Dec, 2025 Read the published version in Archaeological and Anthropological Sciences → Version 1 posted 11 You are reading this latest preprint version Abstract During the Middle and Recent Bronze Age (c. 1350–1150/1100 BCE), the Terramare culture played a crucial role in the development of both regional and interregional trade networks of the Po Plain of northern Italy, particularly through the production and exchange of metal artefacts. While substantial research has focused on the bronze objects themselves, the technical aspects of metal production, such as refining, alloying and recycling methods, remain underexplored. This study addresses this gap by analyzing a series of metallurgical by-products from the Terramara Santa Rosa di Poviglio site, including crucible fragments, and secondary metal remains. Utilizing Digital Microscopy and Scanning Electron Microscopy combined with Energy Dispersive Spectroscopy (SEM-EDS), we investigate the technical practices involved in copper and bronze production at the site. The results indicate the local processing of partially refined copper ingots, intentional alloying of copper and tin, and the recycling of bronze, demonstrating specialised metallurgical expertise. Moreover, these findings suggest that Santa Rosa di Poviglio was deeply integrated into long-distance trade networks, acquiring raw copper and tin for alloying and production of high-quality metal objects. Overall, this research enhances our understanding of Middle Recent Bronze Age metalworking practices and the socio-economic dynamics of the Terramare culture, paving the way for further studies on metallurgical techniques at other Bronze Age sites of the area to explore regional variations and broader economic connections. Terramare culture Bronze Age metallurgy Chaîne opératoire SEM-EDS Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Figure 9 Figure 10 Figure 11 Introduction It is widely accepted that during the Middle and Recent Bronze Age (c. 1350–1150/1100 BCE), the Terramare culture emerged in the Po Plain of northern Italy as a pivotal player in a vast exchange network that connected Central Europe and the Mediterranean (Bernabò Brea et al., 1997 ; Bernabò Brea & Cremaschi, 2004 ; De Marinis, 2011 ; Peroni & Carancini, 1997 ). The significance of this connection is clear in the remarkable similarity of bronze artefacts found across these regions highlighting their role in the formation and spread of a European metallurgical koinè during the Bronze Age (Peroni & Carancini, 1997 ). Additionally, the abundance of high-quality artefacts discovered at the Terramare sites indicate the advanced skills of metal craftspeople. Traditionally, research has predominantly centered on the chrono-typological seriation of metal objects, focusing mainly on their stylistic and functional characteristics (Carancini, 1975 , 1984 ; Carancini & Peroni, 1999 ; Cupitò, 2006 ; Peroni, 1994 ). In the past two decades, however, a surge in chemical and lead isotopic analyses has enriched our understanding on their composition, production methods, and provenance in the Middle and Recent Bronze Age (e.g., Angelini et al., 2015 ; Angelini, 2005 ; Artioli et al., 2016 ; Aspes, 2011 ; Vicenzutto et al., 2015 ). Nevertheless, the focus on artefacts has not been mirrored by archaeometric studies on technical ceramics, metallurgical waste, and crafting by-products. This imbalance restricts our understanding of key aspects of Bronze Age metalworking, such as the diverse techniques of bronze production, raw materials procurement, and their socio-economic implications. For instance, alloying methods can only be thoroughly understood by examining crucibles and by-products, rather than the finished artefacts themselves (e.g., Montes-Landa et al., 2024 ). Within the context of the Terramare culture, some progress has been made through targeted studies, including an analysis of metallic nodules from Santa Caterina Tredossi (Angelini & Artioli, 2006 ), as well as a preliminary archaeometric investigation of crucibles, waste materials, and metals from the settlement of Beneceto Forno del Gallo (Angelini et al., 2009 ), and the analysis of a tin ingot from the settlement of Parma (Cremaschi et al., 2018 ). These individual studies highlight the need for a more comprehensive exploration of Bronze Age metal technology in this key region. Our current understanding of bronze production techniques remains at an early stage, suggesting that further archaeometric research, particularly into metallurgical by-products and waste, could offer critical insights into production methods, resource acquisition, and technological advancements within the Terramare settlements. Given the limited evidence of furnace installations or structures dedicated to metallurgical activities in the Terramare archaeological context (Armigliato, 2017 ), the remains of technical ceramics, crucibles and associated secondary metallurgical by-products are crucial to provide insights into the metallurgical processes involved in copper and bronze production (e.g. Rademakers and Rehren 2016 ). This study analyses a selection of crucible fragments and secondary by-products from the Terramare Santa Rosa di Poviglio site (hereafter TSRP) aiming to identify the metallurgical practices conducted at the site (Fig. 1 ). Specifically, it explores whether these materials were exclusively connected to bronze casting and artefact production, as already widely attested by the presence of fragmented objects and ingots (Bianchi, 2018 and references therein), or served other metallurgical purposes such as copper alloying, recycling, and refining, as well as the types of metals employed. Addressing these questions will provide new insights into the technical practices, production strategies, and socio-economic context of metalworking technologies that remain largely unknown both at a regional and super-regional scale. The high amounts of metal recovered at the site in various forms such as ingots, metal scraps, slags and entire and fragmented artefacts (Bianchi, 2018 ; Cremaschi, Mutti, et al., 2016 ), its strategic location in the hearth of the Po valley, along with its attested importance in the Terramare socio-economic context and its chronological alignment with the zenith of the Terramare culture, make TSRP an ideal candidate to address this gap in knowledge. Archaeological background The Terramare sites are the archaeological remains of banked and moated villages developed in the central alluvial plain of the Po River (N Italy) during the Middle and Recent Bronze Ages (1550 − 1170 cal yr BCE) (Bernabò Brea et al., 1997 ; Cremaschi, 2014 ). This culture reached its apogee at the beginning of the Recent Bronze Age, then underwent a societal collapse followed by population relocation, leading to the abandonment of the villages of the whole region in a few generations (Cardarelli, 2010 ; Cremaschi et al., 2016 ). The Terramare villages are evidence of a complex society, whose subsistence was based on intensive agriculture, pastoralism, and long-distance trade (Barfield, 1994 ; Bernabò Brea et al., 1997 ; Cardarelli, 1997 ). The Terramare-type villages were squared in shape with houses on posts, distributed in regular rows and enclosed inside earthen rampart. They were surrounded by moats connected to the local fluvial network with the purpose to collect water and distribute it to cultivated fields by means of irrigation ditches to sustain agriculture (Cremaschi et al., 2016 ; Cremaschi & Pizzi, 2010 ). Thanks to the extensive excavation campaigns carried out over the past 42 years, the TSRP is one of the best-known Bronze Age sites in Italian protohistory. The site is in the alluvial plain, about 3 km southward from the present-day course of the Po River (Fig. 1 ). Geomorphological evidence suggests that the site was located near a palaeochannel of the Po River, which was active during the lifetime of the Santa Rosa village (Bernabò Brea & Cremaschi, 2004 ). The site consists of two dwelling areas indicated as “Villaggio Piccolo” (that in Italian means ‘Small Village’; hereafter: VP) dating to the Middle Bronze Age (c. 1650–1350 BCE), and “Villaggio Grande” (‘Large Village’; therein: VG), which developed in the later phases of the Middle Bronze Age and in the Recent Bronze Age (Fig. 1 ). Continuous habitation persisted in the VG until the later phases of the Late Bronze Age (Bernabò Brea et al., 1997 ; Bernabò Brea & Cremaschi, 2004 ). The moat separating the VP from the VG is 4m deep and it is part of the complex system of hydraulic structures of the site that has been extensively explored (Cremaschi & Pizzi, 2011 , 2021 ). The metallurgical evidence presented in this paper was recovered from the Recent Bronze Age phases of the VG. Materials and methods Several dozens of Bronze Age metallurgical items were recovered at TSRP, including artefacts, crucible fragments and slags (Bianchi, 2018 ; Pizzi, 2021 ). In this study, we consider 11 specimens coming from the VG area and selected for in-depth analysis: 5 crucible fragments (two of which from the same fragment 115, see Table 1 ), 1 slag (crucible’s slagged surface), and 5 secondary metal by-products (Table 1 ). These specimens were chosen for their representativeness in investigating technical metallurgical processes and their suitability for analysis. Selection criteria included dimensions and structural integrity, as overly brittle specimens were avoided to ensure they withstood the preparation process. To preserve archaeological materials, only fragmented crucibles were considered, and microsamples were extracted from them. The analyses were carried out at the British Museum Department of Scientific Research, using a combination of Digital Microscopy and Scanning Electron Microscopy coupled with Energy Dispersive Spectrometry (SEM-EDS). Following macroscopic investigation, the samples were cut to obtain flat cross-sections using a wet steel bench saw. Then specimens were cold mounted in epoxy resin and the surfaces ground using increasingly finer abrasives and polished down to 1/4µ using diamond paste. Reflected Light Microscopy observations were carried out using the Keyence VHX 5000 microscope. Following carbon coating of the samples, SEM-EDS analyses were carried out at high vacuum using a Hitachi S-3700 Scanning Electron Microscope equipped with an Oxford Inc. EDS. An accelerating voltage of 20 kV was used, with a working distance of 10 to 12 mm and a live time of 90 seconds. To optimise quantitative analyses a cobalt standard was used. The analyses were acquired with the Aztec 5.1 software using standard calibrations. Crucible samples were investigated following the methodology employed by Rademakers and Rehren ( 2016 ) and Rademakers et al. ( 2018 ). The outer ceramic and the inner vitrified zones were compared. The methodology consists of the analysis of 5 different areas for each zone. The area analysed is the visible area at 100x magnification (± 1mm 2 ). Data analysis and visualization were carried out using R version 4.0.3 (R Core Team, 2020 ) and the ggplot2 package (Wickham, 2016 ). Table 1 List of the samples investigated in this study. “VG” stands for Villaggio Grande. Find ID Type SU Year Location OM SEM-EDS 91 Crucible 2932 2002 VG X X 124 Crucible 2518 2002 VG X X 115a Crucible 2790 2001 VG X X 115b Crucible 2790 2001 VG X X 91a Crucible (only slagged surface) 2614 2001 VG X X 149 Crucible and bronze 2960 2002 VG X X 19 Ingot 3107 2004 VG X X 46 Ingot 2379 2000 VG X X 12 Copper 8038 2010 Ditch VG (south) X X 20 Bronze 1049 1999 VG X X 104 Bronze scrap laminae 2430 2000 VG X X Results This section presents the most relevant analytical results, while full results are reported in the Supplementary Materials. The initial part of this section concentrates on the crucible fragments, while the subsequent part focuses on the secondary metallurgical products and by-products. As general consideration, the reader must be aware that most of the considered items show evidence of external weathering in waterlogged conditions. In fact, the whole archaeological site is subject to the fluctuation of the water table and, in some parts, the archaeological sediments were at least seasonally in the saturation zone. Crucible remains Crucible fragments measure between 2 and 4 cm in length, with wall thicknesses ranging from 1 to 2.5 cm. Unfortunately, their small dimensions make it impossible to gather information for reconstructing their original size and shape and, in some cases, distinguish between their inner and outer sides. The samples display a predominantly fine, light-coloured fine matrix with a smooth texture. No fiber-like impressions or elongated fractures and porosity, which could indicate the use of organic temper in the fabric, were identified. Additionally, only minimal millimetric inclusions were observed. All the three commonly identified zones in a crucible wall - externally, a fired ceramic zone; centrally, a bloated zone; and internally, a vitrified ‘crucible slag’ zone (Rademakers et al., 2018 a) - were observed, typical for internally heated crucibles. The crucible interiors exhibit variable vitrification or thermal alteration marks, with layers characterized by bloated and slagged green, grey, and black bubbles, displaying increasing porosity towards the crucible interior, exposed to heat at the interface with the crucible charge (Fig. 2). This vitrification is the result of ceramic melting under high heat exposure and fuel ash contamination. A vast range of metal prills and metal oxide inclusions with various compositions were identified in this vitrified zone (thus a ‘crucible slag’) for all samples (see “Metal prills” section below). All 5 samples show the presence of tin in various forms. It is present in the metallic phase as a constituent of bronze (but not as pure tin metal) or as two different oxides. Tin oxides, identified as “highly euhedral rhomboids or as needles” (Dungworth, 2000 ) were primarily found in bloated and vitrified areas, as well as on the exterior surface of the bronze fragment TSRP20. These oxides are mainly found in clusters across the crucible surfaces, often associated with copper phases, and are absent in other regions. Tin was also identified as a compound resembling malayaite (CaSnO(SiO 4 )), likely formed through the interaction of SnO 2 with Ca-rich pyroxenes/lime-rich crucible slag (Fig. 3 a-d). In some cases, these malayaite-like compounds have a high concentration of iron (TSRP91a, sp. 38–39), which might be due to either the co-occurrence of iron-bearing minerals in the surrounding environment or the substitution of tin by iron. In malayaite, Fe²⁺ or Fe³⁺ ions may substitute for Sn⁴⁺ in the crystal structure because tin and iron have similar ionic radii (similar substitution of iron by tin occurs in the spinel-like oxidation products frequently encountered in crucible slag, e.g. Rademakers et al. 2018 ). This substitution can occur if tin is less abundant, and iron is prevalent in the system. The extent of substitution can vary. Unfortunately, these crystals offer no insight into the specifics of the alloying process, as they can form during both melting and re-melting, as well as during alloying operations (cf. Rademakers and Farci 2018 , and references therein). No traces of cassiterite were found, making it difficult to determine the specific process used at the site to produce bronze. Figure 2 BSE image showing the cross-section of one of the crucibles investigated in the current research (TSRP 124). It shows the full profile of a crucible fragment with bloated layer on the right (crucible interior) and increasingly less vitrified ceramic toward left (exterior, bottom of the sample). Sample TSRP 124 exhibits a noticeable crack on its outer side, filled with metal (Fig. 4). Its wall thickness is about 0.5 cm with the thermally unaltered zone between 1 to 3 millimeters. It appears that the exterior section of the crucible wall is missing from this fragment, with only the internal part being preserved, rather than it representing a complete crucible profile. In some cases, though from later periods, the inner sections of crucibles were lined with additional clay to allow for reuse in subsequent melting processes (e.g. Martinón-Torres & Rehren, 2014 ). These details suggest that this fragment could have been part of such a lining. However, no clear evidence of this practice has yet been reported from the Terramare sites. Alternatively, the exterior ceramic zone of the crucible may have broken off from this particular fragment, leaving only the interior section. It is plausible that the observed crack formed during the heating and melting process, allowing liquid metal to seep into the crack (and possible between the original crucible surface and its secondary lining). However, a definitive assessment remains challenging. In the ceramic bodies of samples TSRP91 and TSRP124, inclusions of monazite ((Ce,La,Nd,Th)PO 4 ), a phosphate mineral rich in light rare earth elements, (LREE), were found (TSRP91, sp. 89, TSRP124, sp. 92). Additionally, another inclusion with high presence of iron and chromium was identified in sample TSRP91 (TSRP91, sp. 181). These minerals reflect the selected ceramic fabric for the crucibles rather than the metallurgical processes conducted therein. Bulk chemical composition and changes This section presents the bulk chemical composition and the observed changes between the crucible ceramic and bloated areas of the investigated crucibles (see Tables in the Supplementary Materials for details). In sample TSRP149, only the bloated areas were preserved. Over these, material primarily composed of bronze and its associated oxide products. This may represent a dross layer formed through oxidation during the casting process (Rademakers et al., 2018 : 1659). Additionally, several green-coloured, corroded regions were observed along the edge of the bloated zone and adjacent to the metal, likely caused by post-depositional corrosion. The main elements detected are SiO 2 , Al 2 O 3 , CaO and FeO. Together, these components make up a total of c. 90% for the ceramic areas and c. 88% for the bloated areas. The data were plotted in ternary diagrams, where three selected oxides were normalised to 100%, excluding other detected elements (Fig. 5). In the SiO₂-Al₂O₃-FeO ternary diagram, the measurements cluster together, showing uniformity both in the ceramic and in the bloated compositions. All the measurements cluster on the SiO 2 -Al 2 O 3 axis showing only slight variability between their contents. In contrast, the SiO₂-Al₂O₃-CaO ternary diagram reveals a more dispersed distribution of measurements, indicating greater variability in composition. Specifically, there is a noticeable and consistent depletion of lime in the bloated areas compared to the ceramic regions. Additionally, copper content shows a significant increase, rising from 0.3 wt% (with a maximum value of 0.4 wt%) in the ceramic areas to 2.1 wt% (with a maximum of 3.5 wt%) in the bloated areas. A slight increase is also observed in the tin content, which rises from 0.2 wt% (with a maximum value of 0.3 wt%) in the ceramic areas to 0.5 wt% (with a maximum value of 0.6 wt%) in the bloated areas (see SM). No charcoal inclusions were identified in the bloated areas. However, indirect evidence of the firing process can be inferred by comparing the crucible ceramic and bloated areas, focusing specifically on lime, alkali and potash content. The relative changes in ratio of oxides to Al 2 O 3 (in wt%) in the bloated areas with respect to the ceramic were measured following the formula from Freestone and Tite ( 1986 ) and Rademakers et al. ( 2018 a:1657): $$\:\frac{\varDelta\:\text{M}\text{e}\text{O}}{\text{A}\text{l}₂\text{O}₃\:}=\frac{\frac{\text{M}\text{e}\text{O}\text{b}\text{l}\text{o}\text{a}\text{t}\text{e}\text{d}}{\text{A}\text{l}₂\text{O}₃\text{b}\text{l}\text{o}\text{a}\text{t}\text{e}\text{d}}-\frac{\text{M}\text{e}\text{O}\text{c}\text{e}\text{r}\text{a}\text{m}\text{i}\text{c}}{\text{A}\text{l}₂\text{O}₃\text{c}\text{e}\text{r}\text{a}\text{m}\text{i}\text{c}}}{\frac{\text{M}\text{e}\text{O}\text{c}\text{e}\text{r}\text{a}\text{m}\text{i}\text{c}}{\text{A}\text{l}₂\text{O}₃\text{c}\text{e}\text{r}\text{a}\text{m}\text{i}\text{c}}}$$ Since alumina is not usually part of the melting charge, normalising metal oxide to Al 2 O 3 avoids distortion from the presence of metals and inclusions. Although the relative changes are minor overall, the comparison of the ceramic and bloated areas (Fig. 6 ) shows moderate increases in sodium (Na₂O) across the samples, particularly in samples TSRP115b (+ 56%) and TSRP115a (+ 33%). Magnesium (MgO) exhibits a similar pattern, with increases in TSRP115b (+ 44%) and TSRP115a (+ 22%). Silica (SiO₂) demonstrates a relatively lower but consistent increase across all samples, with the most pronounced enrichment in sample TSRP115b (+ 24%). In contrast, phosphorus (P₂O ₅) shows moderate depletion in all samples, with reductions ranging from − 50% to -80%. Potash (K₂O) displays varying behaviour. It shows significant increases in sample TSRP91 (+ 29%) and TSRP115b (+ 29%) but remains constant in sample TSRP115a. Lime (CaO) generally shows a notable decrease in all samples, with the strongest depletion occurring in sample TSRP115b (-74%) and TSRP115a (-42%). I ron (FeO) consistently shows a minor increase across all samples, with notable rises in sample TSRP115b (+ 22%) and TSRP115a (+ 20%). Finally, both titanium oxide (TiO₂) and manganese oxide (MnO) remain unchanged across all samples, indicating that they are not significantly affected by the bloating process and interaction with the crucible charge. Interestingly, it is worth noting that differences were identified between two cross-sections (TSRP115a and TSRP115b) of the same crucible (see Rademakers and Rehren 2016 for similar examples). While the general trends are similar, the magnitude of changes is consistently larger in 115b, with greater enrichment in Na₂O, MgO, SiO₂, and K₂O, and a more significant loss of CaO. Overall, the results show how the metallurgical processes led to significant changes in the composition of the crucibles. There is a clear trend of enrichment in sodium, magnesium, silicon, potassium, and iron oxides, while phosphorus and calcium oxides tend to be depleted. These variations likely reflect differences in firing conditions, such as temperature, atmosphere, or material composition (Rademakers & Rehren, 2016 ). As already largely stated by a number of authors (Evans & Tylecote, 1967 ; Misra et al., 1993 ; Rovira, 2007 ; Tylecote, 1982 ; Wood, 2009 ), most of these changes in ratios are due to the chemical interaction of the ceramic body with fuel ash. While this usually involves significant lime contamination too, different wood species produce different ash compositions, resulting in varying crucible slag compositions. Increases in iron oxide content most likely reflect the partitioning of (minor) iron from the metal melt into the crucible slag. Metal prills Numerous prills were identified in each crucible fragment, with 121 analyses conducted in total. All prills are copper-based alloys, and a detailed examination revealed their predominantly spherical shape, indicating their transition to a liquid state during processing. Many prills are heavily corroded, often surrounded by metal oxides. Weathered copper-bearing phases with both spheroidal and lath-like growth morphologies were also identified (see Supplementary Materials for details). The sample TSRP91a contains Cu-Sn prills at various stages of oxidation, distributed throughout the entire cross-section. These features, along with the composition ratios of the matrix, which are similar to those of sample 149, suggest that may have originated from the interaction of melted metal with the crucible surface. Despite these transformations, it is important to recognize that oxidation may also result from fluctuating redox conditions within the crucible during the process. Distinctive prills with elevated tin concentrations were found in the bloated and slagged layers of four samples (TSRP91, TSRP115b, TSRP149, TSRP91a). The tin content ranged from 20.3 wt% (TSRP91, sp. 69) to as high as 94.2 wt% (TSRP91, sp. 67). A summary of the elemental concentrations (Minimum, Maximum, Mean, and Standard Deviation (σ)) across the four samples (91a, 91, 149, 115b) is provided in Table 2 . A comprehensive list of high-tin prills measured in each sample is provided in the SM (Table 14). The presence of high-tin prills provides direct evidence of intentional alloying of copper (or recycled bronze), (Crew and Rehren, 2002 ; Rehren, 2001; Rehren and Pusch, 2012). Traces of iron, nickel, arsenic, antimony, and lead were identified in the majority of the investigated prills, with some prills exhibiting traces of silver. Specifically, iron ranged from 0 to 1.7 wt%, nickel from 0 to 1.0 wt%, arsenic from 0.1 to 0.9 wt% and antimony from 0.5 to 3.0 wt%. Lead concentrations varied between 0 to 5.3 wt%. Interestingly, the metal found in the crack and the prills in crucible TSRP124 are primarily composed of copper, with only small amounts of tin present. Two analyses revealed tin concentrations of 2.2 wt% and 2.3 wt%, while two other analyses showed tin concentrations as low as 0.1 wt%. In addition to this, tin oxides were observed on the superficial inner side of the crucible. Table 2 Summary of the elemental concentrations (Minimum, Maximum, Mean, and Standard Deviation (σ)) across four different samples (91a, 91, 149, 115b). In brackets the number of analyses undertaken. Sample Type Fe Co Ni Cu As Ag Sn Sb Pb 91a (35) Crucible Min 0.1 0.4 54.9 0.1 0.1 20.3 0.5 Max 1.7 0.7 1 78.6 0.9 0.1 42.2 1.7 0.7 Mean 0.50 0.53 0.25 64.95 0.23 0.10 32.95 1.03 0.19 σ 0.39 0.10 0.22 6.93 0.15 0 6.35 0.33 0.12 91 (11) Crucible Min 0.1 0.1 0.3 0.1 21.1 0.5 0.1 Max 0.4 0.9 77.6 0.9 94.2 3 4.1 Mean 0.26 1.40 0.22 60.05 0.26 37.35 1.05 0.85 σ 0.10 0.24 21.91 0.23 20.62 0.69 1.14 149 (2) Crucible Min 37.3 0.1 43 0.5 0.1 Max 56.2 0.1 61.7 1 0.1 Mean 46.75 0.10 52.35 0.75 0.10 σ 13.36 0 13.22 0.35 115b (23) Crucible Min 0.1 0 40.3 0.1 22.7 0.5 0.1 Max 0.5 0.4 73.9 0.3 52.4 1.9 5.3 Mean 0.29 0.20 59.43 0.14 37.32 1.10 1.74 σ 0.14 0.11 6.82 0.06 6.24 0.31 1.16 Secondary metallurgical products and by-products The 5 samples of secondary products investigated exhibited a variety of distinct characteristics in morphology and composition (Fig. 7). The following sections provide an overview of the key structural and compositional features observed in each sample. Two samples (TSRP19 and TSRP46) consist of almost completely oxidised copper alloy (Fig. 7a-b). Both specimens contain numerous round and elongated copper sulphide inclusions of varying dimensions scattered across their surfaces (Fig. 8a-b). In sample TSRP19 (Fig. 8a), the Cu/S ratio of the copper sulphide inclusions is highly consistent, averaging c. 79 wt% Cu and 21 wt% S, with a comparable Cu/S ratio in sample TSRP46. Both samples displayed voids and porosities across the surface (Fig. 9), which may be attributed to the release of gases such as oxygen, carbon monoxide, carbon dioxide, and sulphur dioxide during oxidation of sulphide inclusions in the molten state (see Hauptmann et al., 2016 ). Traces of tin (Sn) were detected in 21 out of 40 analyses for TSRP19, with concentrations ranging from 0.1 wt% to 1.2 wt%, and one outlier measuring 7.2 wt% (SR19, sp. 34 of the SM). In contrast, TSRP46 showed minimal traces of tin, with only 9 out of 25 analyses detecting Sn at levels between 0.1 wt% and 0.2 wt%. Additional trace elements identified in TSRP19 include iron, typically ranging from 0 to 0.9 wt% but up to at 4.9 wt%, zinc, with concentrations between 0 and 2 wt%, while silver ranged from 0 to 0.5 wt%, except for a significant peak at 9.5 wt% (TSRP19, sp. 61). Antimony (0 to 1.7 wt%) and lead (0 to 0.8 wt%) were also present, alongside small traces of arsenic and nickel. TSRP46 displayed similar trace element concentrations, with iron typically ranging from 0 to 1.4 wt% and up to 4.8 wt%, zinc between 0 and 1 wt%, silver from 0 to 0.4 wt%, and lead between 0 and 1.1 wt%. By contrast, only low traces of antimony (a maximum of 0.1 wt%) were detected, while arsenic was identified in the range of 0 to 1.3 wt% and up to 3.1 wt%. Both samples have few inclusions: one metallic inclusion of lead-bismuth (Pb-Bi) was identified in each sample. Lead and bismuth have low solubility in copper and tin alloys, and they tend to segregate into inclusions during solidification. An inclusion of highly oxidised lead was identified in sample TSRP19. Sample TSRP20 is a solid metallic bronze fragment with dendritic, as cast structure (Fig. 7d). It illustrates the typical variation in surface preservation due to corrosion. Two distinct concentric layers can be observed: the outer layer, composed of earth minerals and secondary corrosion products and the inner layer, representing the original surface of the fragment and associated corrosion products, predominantly oxidized copper compounds. The various stages of oxidation of copper and tin compounds observed near the surface reflect the progressive exposure to oxygen in the external environment. The metallic area exhibits expanded regions characterized by a tin bronze composition, revealing a dendritic cored (fern-like) texture characterized by small polygonal grains (α-phase) surrounded by a solution richer in tin (Fig. 10a-b). These dendritic growths are particularly evident in the crystallisation of solid solutions, mostly arise from two-phase alloys (Scott, 2012 ). The tin content varies across the sample, ranging from approximately 0-0.5 wt% in the dendrite cores, to about 25 wt% in the interdendritic zones (Fig. 10b). Due to the substantial difference between these zones, area analyses of approximately 1 mm² were conducted to discern the chemical composition of the alloy. These analyses revealed a bronze alloy composition with an approximate composition of 95.8 wt% Cu and 4.2 wt% Sn, similar to the composition of the casting flash analyzed in sample TSRP104 (cf. below). Several inclusions were identified within the sample, including exogenic globules of copper sulphides in the films around the grains (Fig. 10b). Lead- and sulphur-rich inclusions were also present, likely from sulphide ore minerals residual to raw copper. Oxygen content suggests that partial oxidation has occurred in these sulphide inclusions. Additionally, endogenic inclusions of tin oxides (SnO₂) were found, distributed in the tin-rich zones surrounding the α-grains. Their presence, far from the oxidized surface, along with the partial oxidation of the lead compounds, indicates that the metal underwent high-temperature reactions, suggesting that oxygen exposure likely occurred during alloying or casting of this object. Close to the exterior surface, various copper and tin compounds at different stages of oxidation were identified, with oxidized copper showing oxygen contents ranging from 8.9 wt% to 33.3 wt%. Numerous tin oxides were also present (Images 7 and 8). Low traces of iron (up to 0.1 wt%), zinc (up to 0.2 wt%), arsenic (up to 2.7 wt%), antimony (up to 2.6 wt%), silver (up to 0.9 wt%), and lead (up to 3.6 wt%) were detected throughout the sample. Sample TSRP12 (Fig. 7c) is primarily composed of nearly pure copper, with an average composition of 96.7 wt%, determined through four area analyses (TSRP12, sp. 1, 6, 12, and 19). Scattered across the entire surface several small, mainly round copper sulphide inclusions of varying dimensions were identified, averaging 19 wt% S and 77 wt% Cu (TSRP12, sp. 4, 8, 24–27, 30). Additionally, voids and porosity ranging from a few to several microns were detected throughout the sample. Cubic cuprite crystals were found crystallized within several of these pores. Numerous cuprite inclusions, along with lead- and sulphur-rich inclusions were also observed scattered throughout the sample, likely remnants of the extractive charge. Traces of iron were identified ranging from 0.1 to 0.8 wt%. Zinc concentrations varied between 0 and 0.5 wt%. Low traces of silver (up to 0.2 wt%) and antimony (up to 0.6 wt%) were detected. Lead was found in concentrations ranging from 0 to 1 wt%. Sample TSRP104 is characterized by an amalgamation of flat lamellae, with varying lengths and a thickness range between 100 and 200 µm (Fig. 7e). Although a significant portion of these lamellae exhibited pronounced oxidation and weathering on their outer surfaces, 31 analyses were conducted on the low-oxidized areas of these lamellae (Fig. 11a-b), revealing a relatively uniform composition, with an average of 94.3 wt% copper (Cu) and 5.7 wt% tin (Sn). Copper concentrations ranged from 94.9 wt% to 90.3 wt% (σ = 1.3), while tin content varied from 7.4 wt% to 3.1 wt% (σ = 1.2). Low traces of iron, nickel, zinc, and silver were identified with concentrations up to 0.1–0.2 wt%. Arsenic, antimony, and lead showed similar values, with concentrations up to 0.3–0.4 wt%. Discussion The analysis of the samples investigated has revealed a variety of activities associated with copper and bronze production at the site of TSRP. These findings provide valuable insights into different stages of bronze-related processes, including copper refining, tin alloying for bronze production, and the recycling of bronze materials. In this section, the data presented in the results section is discussed, focusing on how these processes were carried out and on their broader implications. Copper refining The high concentration of copper sulphide inclusions and the presence of numerous voids and porosities observed in samples TSRP19 and TSRP46 suggest that these specimens likely represent (parts of) copper ingots composed of raw or (partially) refined copper. These features align with those typically found in ancient copper bars and ingots, such as the Late Bronze Age copper oxhide ingots from the Uluburun shipwreck (Hauptmann, 2020 , p. 438; Hauptmann et al., 2016 , pp. 753–754). The squared shapes of the fragments (Fig. 7a-b and Supplementary Materials) further suggest their classification as ingot (fragments). Such characteristics suggest that the copper ingots were not fully refined and were possibly acquired in this semi-processed state before undergoing additional on-site refinement. This scenario is consistent with ancient metallurgical practices, where ingots with impurities were refined closer to the final point of use or manufacturing (Hauptmann et al., 2002 ). Sample TSRP12 likely represents a later stage in the copper refining chaîne opératoire . Its small, predominantly round copper sulphide inclusions, present in lower amounts than in the other samples, are likely remnants which were supposed to be removed. This indicates that TSRP12 may be an incompletely refined copper derived from more copper sulphide-rich ingots. Further along in the metallurgical sequence is the cast bronze fragment TSRP20, which contains even lower amounts of copper sulphide inclusions, possibly indicating that it is a newly cast tin-bronze alloy. These sulphide inclusions, mainly dispersed along the films surrounding the grains, cannot recrystallize during working or annealing and offer valuable insights into the alloy's transition from the cast to the worked state (Scott & Schwab, 2019 ). The consistent presence of copper sulphides, lead- and sulphur- inclusions, alongside trace elements such as As, Sb, Ni, Ag, Zn, and Pb in samples TSRP19, TSRP46, TSRP12, and TSRP20, suggests a common origin for the metal, possibly from sulfidic and/or sulfosalt ore deposits. These characteristics likely point to consumption at TSRP of copper resulting from the exploitation of the fahlerz-type deposits in the Alpine area, located about 150 km north, which were heavily mined during the Late Bronze Age. (AAcP, 2018 ; Addis, 2013 ; Artioli et al., 2016 ; Canovaro et al., 2019 ; Ling et al., 2019 ) Intentional tin-alloying The presence of high-tin prills affords key evidence for intentional tin-alloying (e.g. Crew & Rehren, 2002 ; Rademakers and Farci 2018 , Rademakers et al. 2018 a). During the bronze alloying process prills rich in tin reflect incomplete mixing products which may remain trapped in the vitrified crucible interior. The detection of high-tin prills in specific crucible regions indicates an incomplete amalgamation of copper and tin, serving as tangible evidence for the active alloying of copper or recycled bronze with a tin component. This phenomenon has been extensively investigated and experimentally confirmed by various researchers (e.g. Rademakers and Farci 2018 , and references therein). The remelting of existing bronze leads to prills with a tin content either lower or equal to that of the recycled bronze. This is because tin, having a higher affinity to oxygen than copper, tends to be depleted from trapped prills under (mildly to strongly) oxidising conditions (e.g. Dungworth, 2000 ; Kearns et al., 2010 ; Rademakers & Rehren, 2016 ). When alloying copper or recycled bronze with tin, prills can exhibit any composition between pure copper and tin. It is important to note that no objects with such high tin content have been identified in the Terramare archaeological record and therefore these high-tin prills cannot indicate recycling. Therefore, in the process of producing a low-tin bronze, these high tin prills represent an intermediate product of the alloying process and their presence trapped in the crucible bloated and slagged surfaces are incidental. However, the absence of tin-rich prills in other examined cross-sections does not preclude the examined crucible's use for active alloying or evidence of recycling. This could be due to prills forming only when a complete reaction did not occur in the analyzed area, or because the distribution of tin during alloying is not uniform across the crucible. This is underscored by the analysis of two cross-sections from the same crucible (TSRP115a and TSRP115b), where only the second section revealed high-tin prills, highlighting the variability of process conditions during crucible alloying (as emphasized by Rademakers and Rehren 2016 ). The presence of tin oxides combined with the low tin content in the metal prills trapped inside the crucible wall of sample TSRP124 suggests (at least) two possible scenarios, not necessarily mutually exclusive. One hypothesis is that the crucible was used previously for bronze alloying or melting. In this scenario, tin oxides found in the crucible may be residues from earlier alloying operations, where the tin was oxidized and left behind. The crucible was used previously to deal with Cu-Sn alloys and in its final use, only copper may have been melted in the crucible. Another plausible explanation is that the crucible was used for actively alloying copper and tin to produce bronze and during this process, the crack formed before complete mixing of the metals. As a result, the copper-rich metal that seeped through the crack did not fully mix with the tin in the charge, resulting in the low tin content in the seeped metal. At the same time, the unalloyed tin likely oxidized, forming the tin oxides observed inside the crucible. Unfortunately, it was not possible to identify the source of tin used at the site, as no residual cassiterite grains were observed in the samples. The prills rich in tin do not provide evidence of the source of tin adopted either in metallic or mineral form (cassiterite, SnO₂). It is known that tin in the Middle Bronze Age (Cremaschi et al., 2018 ) Late Bronze Age (Berger et al., 2022 ; Powell et al., 2022 ) was traded as ingots, but cassiterite is also common in the Alps, making both sources plausible. Cassiterite introduced into a crucible with copper might be reduced to metallic tin before interacting with the copper (Rademakers and Farci, 2018 , experiments 17–18). Indeed, it is impossible to determine whether newly formed tin features originated from metal or ore (such as cassiterite) – although tin oxide inclusions enriched in elements such as tantalum and niobium are indicative of cassiterite use (see also Figueiredo et al., 2017 ; Renzi & Rovira, 2016 ). Several methods could have been employed and the more likely are a) co-melting of metallic copper and tin directly, b) cementing metallic copper with natural tin oxide ore (cassiterite) and c) recycling existing bronze, potentially with the addition of copper or tin metal/ore to control the alloy. Other, less likely methods in this context include: d) the natural alloying of Cu-Sn ore (stannite, Cu 2 FeSnS 4 ) and e) the co-smelting of Cu ore (azurite, Cu 3 (CO 3 ) 2 (OH) 2 , malachite, Cu 2 CO 3 (OH) 2 ) and Sn ore (cassiterite, SnO₂). In case d) a higher amount of iron would be expected in the crucible slag. Similarly, in case e), more residue from the copper ore would be expected, especially given that the ore used appears to be fahlerz , which would result in some “smelting slag” formation within the crucible (Montes-Landa et al., 2024 for a more detailed discussion; see F. W. Rademakers & Farci, 2018 ). Bronze recycling The flat laminae observed in sample TSRP104 can be interpreted as by-products of the casting process, commonly referred to as flashes. They typically accumulate at the parting lines of a bivalve mould, where misalignments or gaps between the mould halves, possibly caused by the metal’s weight pushing the valves apart, allow excess material to escape and accumulate requiring post-casting removal. The relatively uniform composition of the laminae, which shows a low-tin copper alloy, makes it plausible that these remnants were deliberately collected from one or more objects made of the same alloy for reuse or recycling in subsequent casting processes. The practices of intentional collection and recycling of bronze materials, including small pieces like these lamellae, were likely driven by the need to minimize waste and maximize the utility of existing materials. This suggests a relatively high value placed on bronze, likely in a context of relatively limited access to raw materials. Bonze production at the Terramara of Poviglio Overall, these pieces of evidence provide a more nuanced understanding of both the technological and social aspects of metallurgy in one of the most important areas of the Italian peninsula during the Middle and Recent Bronze Ages. Several stages of the bronze production chaîne opératoire have been identified at the site: Refining of raw copper ingots; Active alloying (low-tin bronze production); Bronze casting (though not directly studied in the current research, many metal objects and moulds found on site attest to this process, see Introduction); Bronze recycling. These stages indicate that local metallurgists possessed specialised knowledge of copper, tin, and bronze properties, as well as expertise in the sequence needed to transform raw copper ingots into pure copper and eventually bronze. The discovery of partially refined copper ingots indicates that metallurgists acquired unfinished raw material, rather than opting for finished copper or bronze ingots ready for casting. It can be noted that refining and alloying could in principle take place during a single metallurgical operation (with the removal of dross prior to casting), and the choice for initial refining reflects a particular technological choice which should be compared to other contemporaneous evidence. It may relate to a preference of ‘testing’ materials before alloying, perhaps as a response to variations in raw copper composition arriving at settlement sites. The acquisition of raw copper and the evidence of tin alloying at the site implies that tin, either in a metallic or mineral form, had to be acquired separately too. Since copper and tin often came from different regions and the site of TSRP is located in a territory devoid of any copper and tin ore deposits, the implication is that metallurgists at the site of TSRP, or intermediaries who facilitated the exchange of raw materials between regions, had to participate in distinct or interconnected medium- and long-distance procurement routes for each metal and manage the acquisition and transportation of raw materials before engaging in the production of bronze. This work, through evidence of diverse metallurgical practices carried out at the site, allows to highlight the complex and intricate system of metal production and trade networks within the context of the Bronze Age Terramare culture. Future research should focus on extending this investigation on a larger scale, examining specializations in metal and alloy production at different sites with the aim to explore the variability of specialisations and practices at regional and super-regional scale and provide further insight into the economic and social dynamics of Recent Bronze Age communities and trade networks. Conclusions This study has provided a detailed examination of the metallurgical practices at the TSRP during the Middle and Recent Bronze Age, shedding light on the complex and multifaceted processes of copper and bronze production. The findings reveal a series of specialised metallurgical techniques of the bronze production chaîne opératoire , including the refining of raw copper ingots, the intentional alloying of copper and tin to produce (low-)tin bronze, and the recycling of bronze materials, each indicative of a high level of technical expertise and specialised metallurgical knowledge. The discovery of partially refined copper ingots suggests that raw copper was acquired in an unfinished state and processed locally, rather than being imported as a fully refined product. This, along with evidence of active tin-alloying, implies that tin had to be acquired separately, underscoring the site's reliance on long-distance procurement networks. Given that copper and tin deposits were not locally available, these findings reinforce Poviglio's deep integration into interregional trade systems, facilitating the acquisition and transformation of raw materials into high-quality metal objects. Furthermore, the presence of recycled bronze material reflects the importance of metal as a resource and the metallurgists' commitment to minimizing waste and maximizing the utility of available materials in an environment with limited access to raw materials. Future research should extend this investigation to other sites of the Terramare culture to explore regional and super-regional variability in metal production. By examining the technological and socio-economic implications of metallurgical practices at different sites, we can gain deeper insights into the role of the Terramare culture in shaping the trade networks and economic systems of the Middle and Late Bronze Age, as well as their broader social dynamics. Moreover, further analysis of metallurgical by-products, including slag and crucible fragments, will be essential for reconstructing the full spectrum of metalworking practices at these sites. Declarations Author Contribution A.A. and F.W.R. conceptualized the study and developed the research framework. A.A. carried out the archaeological sampling and laboratory analyses. A.A. and F.W.R. interpreted the metallurgical data and prepared the data visualizations. A.Z. and M.C. provided the archaeological context and reviewed the relevant archaeological and historical literature. A.A. and A.Z. drafted the main manuscript text. All authors contributed to the interpretation of the results, revised the manuscript, and approved the final version. Acknowledgement The archaeological excavation of the Terramara of Santa Rosa di Poviglio is going on since 1984 under the direction of MC and since 2019 of AZ. The Italian Ministry of Culture (MiC) released the permits for archaeological excavation and sampling archaeological materials. We would like to thank the Municipality of Poviglio and the collaborators of the Museo della Terramara for the continuous support. The archaeological investigation at Santa Rosa di Poviglio was supported by the University of Milano (Fondi Speciali per le Ricerche Archeologiche), the Municipality of Poviglio and Coopsette. Additional contribution comes from an action of the National Recovery and Resilience Plan (NRRP): Cultural Heritage Active Innovation for Sustainable Society (CHANGES) Project, funded by the European Union – NextGenerationEU, under the National Recovery and Resilience Plan (NRRP) Mission 4, Component 2, Investment Line 1.3. References AAcP. (2018). Alpine Archaeocopper Project. [Dataset]. http://www.geoscienze. unipd.it/aacp/welcome.html. Addis, A. (2013). Late Bronze Age metallurgy in the Italian Eastern Alps: Copper smelting slags and mine exploitation [PhD Thesis]. Università di Trento. Angelini, A., Angelini, I., Artioli, G., Nimis, P., & Villa, I. M. (2015). Tipologia e archeometria dei bronzi di Castel de Pedena (San Gregorio nelle Alpi, Belluno). In G. Leonardi & V. Tinè (Eds.), Preistoria e Protostoria del Veneto. (Crocetta del Montello (TV), Italy, Vol. 2, pp. 881–886). Grafiche Antiga,. Angelini, I. (2005). 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Ancient metals: Microstructure and metallurgy. Volume I: Vol. I. Copper and copper alloys . CSP: Conservation Science Press. Scott, D. A., & Schwab, R. (2019). Metallography in Archaeology and Art . Springer International Publishing. Tylecote, R. F. (1982). The Late Bronze Age: Copper and bronze metallurgy at Enkomi and Kition. In J. D. Muhly, R. Maddin, & V. Karageorghis (Eds.), Early Metallurgy in Cyprus, 4000– 500 BC (pp. 81–100). Pierides Foundation. Vicenzutto, D., Dalla Longa, E., Angelini, I., Artioli, G., Nimis, P., & Villa, I. M. (2015). Manufatti in bronzo del sito arginato di Fondo Paviani (Verona)–Scavi Università di Padova 2007–2012. Inquadramento tipocronologico e analisi archeometriche. Studi Di Preistoria e Protostoria—2—Preistoria e Protostoria Del Veneto. , 833–838. Wickham, H. (2016). ggplot2: Elegant graphics for data analysis . springer. Wood, N. (2009). Some implications of the use of wood ash in Chinese stoneware glazes. In A. Shortland, I. C. Freestone, & T. Rehren (Eds.), From Mine to Microscope. Advances in the Study of Ancient Technology (pp. 51–60). Oxbow Books. Additional Declarations No competing interests reported. Supplementary Files Armigliatoetal.DecodingbronzeproductionatPoviglioSupplementarymaterials.docx Cite Share Download PDF Status: Published Journal Publication published 05 Dec, 2025 Read the published version in Archaeological and Anthropological Sciences → Version 1 posted Editorial decision: Revision requested 10 Sep, 2025 Reviews received at journal 26 May, 2025 Reviews received at journal 21 May, 2025 Reviews received at journal 20 May, 2025 Reviewers agreed at journal 06 May, 2025 Reviewers agreed at journal 06 May, 2025 Reviewers agreed at journal 06 May, 2025 Reviewers invited by journal 06 May, 2025 Editor assigned by journal 02 May, 2025 Submission checks completed at journal 02 May, 2025 First submitted to journal 01 May, 2025 You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. 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Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-6572450","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":452894413,"identity":"96ff8702-3711-4976-84f7-d900b11b39ec","order_by":0,"name":"Alessandro Armigliato","email":"data:image/png;base64,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","orcid":"","institution":"British Museum","correspondingAuthor":true,"prefix":"","firstName":"Alessandro","middleName":"","lastName":"Armigliato","suffix":""},{"id":452894414,"identity":"7af6e60c-7f5a-4e78-88a7-9f804a69d7c9","order_by":1,"name":"Frederik W. Rademakers","email":"","orcid":"","institution":"British Museum","correspondingAuthor":false,"prefix":"","firstName":"Frederik","middleName":"W.","lastName":"Rademakers","suffix":""},{"id":452894415,"identity":"67b69451-dc49-4bb7-a751-6550a85b988a","order_by":2,"name":"Andrea Zerboni","email":"","orcid":"","institution":"University of Milan","correspondingAuthor":false,"prefix":"","firstName":"Andrea","middleName":"","lastName":"Zerboni","suffix":""},{"id":452894416,"identity":"0ef26d5e-bf2b-448b-a058-3c3e8141293f","order_by":3,"name":"Mauro Cremaschi","email":"","orcid":"","institution":"University of Milan","correspondingAuthor":false,"prefix":"","firstName":"Mauro","middleName":"","lastName":"Cremaschi","suffix":""}],"badges":[],"createdAt":"2025-05-01 14:23:06","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-6572450/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-6572450/v1","draftVersion":[],"editorialEvents":[{"content":"https://doi.org/10.1007/s12520-025-02357-6","type":"published","date":"2025-12-05T15:56:55+00:00"}],"editorialNote":"","failedWorkflow":false,"files":[{"id":82452730,"identity":"0795e1ce-80bf-4ba6-b563-d88ffe28a83b","added_by":"auto","created_at":"2025-05-11 10:20:09","extension":"jpg","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":157848,"visible":true,"origin":"","legend":"\u003cp\u003eLocation of the TSRP site in Italy (A) and (B) in the central Po Plain in the context of the Terramare culture; key of (B): 1, pre-Quaternary formations; 2, Alpine Pleistocene glacial deposits; 3, Pleistocene deposits at the foot of the Apennine; 4, Pre-Holocene terraces; 5, alluvial plain; 6, sites belonging to the Terramare culture; 7, Terramara Santa Rosa di Poviglio. (C) Simplify map of the TSRP indicating the Villaggio Grande, Villagggio Piccolo, moats and investigated areas; the position of (D) is also reported. (D) Detailed map of the area excavated between the southern limit of the VG settlement and the moat indicating the position of findings discussed in this work; only one sample fall outside from this area and is reported in (C). Key of (D): 1, posthole alignments (huts area); 2, position of investigated samples; 3, VG moat; 4, canals; 5, water wells.\u003c/p\u003e","description":"","filename":"1.jpg","url":"https://assets-eu.researchsquare.com/files/rs-6572450/v1/975ee505c4e7020837fb6da2.jpg"},{"id":82452735,"identity":"561b5307-d441-4e09-a455-5cfb9f1dd8e4","added_by":"auto","created_at":"2025-05-11 10:20:09","extension":"jpg","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":136317,"visible":true,"origin":"","legend":"\u003cp\u003eBSE image showing the cross-section of one of the crucibles investigated in the current research (TSRP 124). It shows the full profile of a crucible fragment with bloated layer on the right (crucible interior) and increasingly less vitrified ceramic toward left (exterior, bottom of the sample).\u003c/p\u003e","description":"","filename":"2.jpg","url":"https://assets-eu.researchsquare.com/files/rs-6572450/v1/9c91013efbd368095de07bd7.jpg"},{"id":82453396,"identity":"fdee9325-52b4-41af-9e42-08a1cb95ebea","added_by":"auto","created_at":"2025-05-11 10:28:08","extension":"jpg","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":206879,"visible":true,"origin":"","legend":"\u003cp\u003eBSE images displaying (a-c) SnO₂ clusters in rhomboid and needle-like shapes (white), d) clusters of malayaite compounds. (a) TSRP115a; b) TSRP91a; c) and d) TSRP 149)\u003c/p\u003e","description":"","filename":"3.jpg","url":"https://assets-eu.researchsquare.com/files/rs-6572450/v1/1205cbc6135007c51aae2de6.jpg"},{"id":82453402,"identity":"295fe9c2-490f-4f6c-8fed-fe86498c1cec","added_by":"auto","created_at":"2025-05-11 10:28:09","extension":"jpg","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":75500,"visible":true,"origin":"","legend":"\u003cp\u003eReflected Light micrographs showing the cross section (a) and the detail of the crack filled with metal, looking at the “exterior” (b) in sample TSRP124.\u003c/p\u003e","description":"","filename":"4.jpg","url":"https://assets-eu.researchsquare.com/files/rs-6572450/v1/04a62f85843e3911daee0311.jpg"},{"id":82453405,"identity":"56cf00b1-a7e2-4925-aa9d-772bd61aaa50","added_by":"auto","created_at":"2025-05-11 10:28:10","extension":"jpg","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":69755,"visible":true,"origin":"","legend":"\u003cp\u003eTernary plots for ceramic (green) and bloated (red) composition in the a) SiO\u003csub\u003e2\u003c/sub\u003e- Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e-FeO and b) SiO\u003csub\u003e2\u003c/sub\u003e-Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e-CaO ternary systems (diagrams after Hall \u0026amp; Insley, 1933; Muan, 1957).\u003c/p\u003e","description":"","filename":"5.jpg","url":"https://assets-eu.researchsquare.com/files/rs-6572450/v1/872f5a0b68c0698845a7f488.jpg"},{"id":82452731,"identity":"5ba5c9bb-19a9-453e-8fee-dd16d858cb0c","added_by":"auto","created_at":"2025-05-11 10:20:09","extension":"jpg","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":67539,"visible":true,"origin":"","legend":"\u003cp\u003eBinary plots showing the relative change in the ratios CaO/Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e vs Na\u003csub\u003e2\u003c/sub\u003eO/Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e, MgO/Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e, P\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e5\u003c/sub\u003e/Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e, K\u003csub\u003e2\u003c/sub\u003eO/Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3, \u003c/sub\u003eSiO\u003csub\u003e2\u003c/sub\u003e/Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3 \u003c/sub\u003eand FeO/ Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e between crucible ceramic and bloated areas. Each point is an average of 5 analyses.\u003c/p\u003e","description":"","filename":"6.jpg","url":"https://assets-eu.researchsquare.com/files/rs-6572450/v1/e3bb99425977d3999773b613.jpg"},{"id":82452734,"identity":"b340b8c3-8065-40d6-817d-9daf818f687b","added_by":"auto","created_at":"2025-05-11 10:20:09","extension":"jpg","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":100769,"visible":true,"origin":"","legend":"\u003cp\u003eReflected Light images showing the cross-sections of the secondary metallurgical products and by-products investigated: a) TSRP19; b) TSRP46; c) TSRP12; d) TSRP20; e) TSRP104.\u003c/p\u003e","description":"","filename":"7.jpg","url":"https://assets-eu.researchsquare.com/files/rs-6572450/v1/a22a3dd3b5bd3092b36e7efd.jpg"},{"id":82452767,"identity":"87ad6be9-eace-4be3-8372-c24fd5144599","added_by":"auto","created_at":"2025-05-11 10:20:10","extension":"jpg","order_by":8,"title":"Figure 8","display":"","copyAsset":false,"role":"figure","size":114852,"visible":true,"origin":"","legend":"\u003cp\u003ea-b (above) BSE images showing the round and elongated copper sulphide inclusions of varying dimensions scattered across sample TSRP19 (a) and TSRP46 (b).\u003c/p\u003e","description":"","filename":"8.jpg","url":"https://assets-eu.researchsquare.com/files/rs-6572450/v1/366005843f9aa5460426f90e.jpg"},{"id":82453442,"identity":"5fbe870a-8a8e-4c21-a7b2-0b6812066abc","added_by":"auto","created_at":"2025-05-11 10:36:09","extension":"jpg","order_by":9,"title":"Figure 9","display":"","copyAsset":false,"role":"figure","size":46482,"visible":true,"origin":"","legend":"\u003cp\u003e(below) BSE image showing voids and pores potentially caused by the release of gases like oxygen, carbon monoxide, carbon dioxide, and sulfur dioxide during the oxidation of sulfide inclusions in the molten phase. Sample TSRP46.\u003c/p\u003e","description":"","filename":"9.jpg","url":"https://assets-eu.researchsquare.com/files/rs-6572450/v1/3c6a53d4b0de9f348cf7d4f0.jpg"},{"id":82452736,"identity":"ed3103b6-c6f8-4007-9616-fa46470a0800","added_by":"auto","created_at":"2025-05-11 10:20:09","extension":"jpg","order_by":10,"title":"Figure 10","display":"","copyAsset":false,"role":"figure","size":95538,"visible":true,"origin":"","legend":"\u003cp\u003eBSE images showing a) the dendritic, as cast structure, of the solid metallic fragment TSRP20, and b) the small polygonal grains (α-phase) surrounded by exogenic globules of copper sulphides (sp. 31) and by solutions richer in tin (sp. 33 and 34). The tin content varies across the sample, ranging from approximately 0-0.5 wt% in the dendrite cores, to about 25 wt% in the inter-dendritic zones.\u003c/p\u003e","description":"","filename":"10.jpg","url":"https://assets-eu.researchsquare.com/files/rs-6572450/v1/7a5d9e6730ceb0155fc5196e.jpg"},{"id":82452765,"identity":"413c4032-e878-4b06-b35f-31c643600f31","added_by":"auto","created_at":"2025-05-11 10:20:10","extension":"jpg","order_by":11,"title":"Figure 11","display":"","copyAsset":false,"role":"figure","size":108951,"visible":true,"origin":"","legend":"\u003cp\u003eBSE images illustrating: (a) a close-up of the flat lamellae within sample TSRP104; and (b) a detailed view contrasting a low-oxidized copper area (sp. 106, light grey) with an oxidized copper area (sp. 107, grey), both surrounded by heavily oxidized and weathered outer surfaces (dark grey).\u003c/p\u003e","description":"","filename":"11.jpg","url":"https://assets-eu.researchsquare.com/files/rs-6572450/v1/07650c2feb5da9c2623a4184.jpg"},{"id":97723742,"identity":"bf0ec125-0021-4bc5-b898-d2e2ceefe18f","added_by":"auto","created_at":"2025-12-08 16:00:57","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":2036310,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-6572450/v1/743d7c82-a223-464a-b930-ee072dda52f8.pdf"},{"id":82452771,"identity":"b43c96ad-019f-444f-aafe-a2206657b1cd","added_by":"auto","created_at":"2025-05-11 10:20:11","extension":"docx","order_by":0,"title":"","display":"","copyAsset":false,"role":"supplement","size":18493889,"visible":true,"origin":"","legend":"","description":"","filename":"Armigliatoetal.DecodingbronzeproductionatPoviglioSupplementarymaterials.docx","url":"https://assets-eu.researchsquare.com/files/rs-6572450/v1/0ab2b165370eb8c2f3517682.docx"}],"financialInterests":"No competing interests reported.","formattedTitle":"Decoding bronze production at Terramara Santa Rosa di Poviglio site (Bronze Age, N Italy): Insights from secondary production waste","fulltext":[{"header":"Introduction","content":"\u003cp\u003eIt is widely accepted that during the Middle and Recent Bronze Age (c. 1350\u0026ndash;1150/1100 BCE), the Terramare culture emerged in the Po Plain of northern Italy as a pivotal player in a vast exchange network that connected Central Europe and the Mediterranean (Bernab\u0026ograve; Brea et al., \u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e1997\u003c/span\u003e; Bernab\u0026ograve; Brea \u0026amp; Cremaschi, \u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e2004\u003c/span\u003e; De Marinis, \u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e2011\u003c/span\u003e; Peroni \u0026amp; Carancini, \u003cspan citationid=\"CR46\" class=\"CitationRef\"\u003e1997\u003c/span\u003e). The significance of this connection is clear in the remarkable similarity of bronze artefacts found across these regions highlighting their role in the formation and spread of a European metallurgical \u003cem\u003ekoin\u0026egrave;\u003c/em\u003e during the Bronze Age (Peroni \u0026amp; Carancini, \u003cspan citationid=\"CR46\" class=\"CitationRef\"\u003e1997\u003c/span\u003e). Additionally, the abundance of high-quality artefacts discovered at the Terramare sites indicate the advanced skills of metal craftspeople.\u003c/p\u003e \u003cp\u003eTraditionally, research has predominantly centered on the chrono-typological seriation of metal objects, focusing mainly on their stylistic and functional characteristics (Carancini, \u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e1975\u003c/span\u003e, \u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e1984\u003c/span\u003e; Carancini \u0026amp; Peroni, \u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e1999\u003c/span\u003e; Cupit\u0026ograve;, \u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e2006\u003c/span\u003e; Peroni, \u003cspan citationid=\"CR45\" class=\"CitationRef\"\u003e1994\u003c/span\u003e). In the past two decades, however, a surge in chemical and lead isotopic analyses has enriched our understanding on their composition, production methods, and provenance in the Middle and Recent Bronze Age (e.g., Angelini et al., \u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e2015\u003c/span\u003e; Angelini, \u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e2005\u003c/span\u003e; Artioli et al., \u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e2016\u003c/span\u003e; Aspes, \u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e2011\u003c/span\u003e; Vicenzutto et al., \u003cspan citationid=\"CR59\" class=\"CitationRef\"\u003e2015\u003c/span\u003e). Nevertheless, the focus on artefacts has not been mirrored by archaeometric studies on technical ceramics, metallurgical waste, and crafting by-products. This imbalance restricts our understanding of key aspects of Bronze Age metalworking, such as the diverse techniques of bronze production, raw materials procurement, and their socio-economic implications. For instance, alloying methods can only be thoroughly understood by examining crucibles and by-products, rather than the finished artefacts themselves (e.g., Montes-Landa et al., \u003cspan citationid=\"CR43\" class=\"CitationRef\"\u003e2024\u003c/span\u003e). Within the context of the Terramare culture, some progress has been made through targeted studies, including an analysis of metallic nodules from Santa Caterina Tredossi (Angelini \u0026amp; Artioli, \u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e2006\u003c/span\u003e), as well as a preliminary archaeometric investigation of crucibles, waste materials, and metals from the settlement of Beneceto Forno del Gallo (Angelini et al., \u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e2009\u003c/span\u003e), and the analysis of a tin ingot from the settlement of Parma (Cremaschi et al., \u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e2018\u003c/span\u003e). These individual studies highlight the need for a more comprehensive exploration of Bronze Age metal technology in this key region. Our current understanding of bronze production techniques remains at an early stage, suggesting that further archaeometric research, particularly into metallurgical by-products and waste, could offer critical insights into production methods, resource acquisition, and technological advancements within the Terramare settlements.\u003c/p\u003e \u003cp\u003eGiven the limited evidence of furnace installations or structures dedicated to metallurgical activities in the Terramare archaeological context (Armigliato, \u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e2017\u003c/span\u003e), the remains of technical ceramics, crucibles and associated secondary metallurgical by-products are crucial to provide insights into the metallurgical processes involved in copper and bronze production (e.g. Rademakers and Rehren \u003cspan citationid=\"CR52\" class=\"CitationRef\"\u003e2016\u003c/span\u003e). This study analyses a selection of crucible fragments and secondary by-products from the Terramare Santa Rosa di Poviglio site (hereafter TSRP) aiming to identify the metallurgical practices conducted at the site (Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e). Specifically, it explores whether these materials were exclusively connected to bronze casting and artefact production, as already widely attested by the presence of fragmented objects and ingots (Bianchi, \u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e2018\u003c/span\u003e and references therein), or served other metallurgical purposes such as copper alloying, recycling, and refining, as well as the types of metals employed. Addressing these questions will provide new insights into the technical practices, production strategies, and socio-economic context of metalworking technologies that remain largely unknown both at a regional and super-regional scale.\u003c/p\u003e \u003cp\u003eThe high amounts of metal recovered at the site in various forms such as ingots, metal scraps, slags and entire and fragmented artefacts (Bianchi, \u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e2018\u003c/span\u003e; Cremaschi, Mutti, et al., \u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e2016\u003c/span\u003e), its strategic location in the hearth of the Po valley, along with its attested importance in the Terramare socio-economic context and its chronological alignment with the zenith of the Terramare culture, make TSRP an ideal candidate to address this gap in knowledge.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e\n\u003ch3\u003eArchaeological background\u003c/h3\u003e\n\u003cp\u003eThe Terramare sites are the archaeological remains of banked and moated villages developed in the central alluvial plain of the Po River (N Italy) during the Middle and Recent Bronze Ages (1550\u0026thinsp;\u0026minus;\u0026thinsp;1170 cal yr BCE) (Bernab\u0026ograve; Brea et al., \u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e1997\u003c/span\u003e; Cremaschi, \u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e2014\u003c/span\u003e). This culture reached its apogee at the beginning of the Recent Bronze Age, then underwent a societal collapse followed by population relocation, leading to the abandonment of the villages of the whole region in a few generations (Cardarelli, \u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e2010\u003c/span\u003e; Cremaschi et al., \u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e2016\u003c/span\u003e). The Terramare villages are evidence of a complex society, whose subsistence was based on intensive agriculture, pastoralism, and long-distance trade (Barfield, \u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e1994\u003c/span\u003e; Bernab\u0026ograve; Brea et al., \u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e1997\u003c/span\u003e; Cardarelli, \u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e1997\u003c/span\u003e). The Terramare-type villages were squared in shape with houses on posts, distributed in regular rows and enclosed inside earthen rampart. They were surrounded by moats connected to the local fluvial network with the purpose to collect water and distribute it to cultivated fields by means of irrigation ditches to sustain agriculture (Cremaschi et al., \u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e2016\u003c/span\u003e; Cremaschi \u0026amp; Pizzi, \u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e2010\u003c/span\u003e).\u003c/p\u003e \u003cp\u003eThanks to the extensive excavation campaigns carried out over the past 42 years, the TSRP is one of the best-known Bronze Age sites in Italian protohistory. The site is in the alluvial plain, about 3 km southward from the present-day course of the Po River (Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e). Geomorphological evidence suggests that the site was located near a palaeochannel of the Po River, which was active during the lifetime of the Santa Rosa village (Bernab\u0026ograve; Brea \u0026amp; Cremaschi, \u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e2004\u003c/span\u003e). The site consists of two dwelling areas indicated as \u0026ldquo;Villaggio Piccolo\u0026rdquo; (that in Italian means \u0026lsquo;Small Village\u0026rsquo;; hereafter: VP) dating to the Middle Bronze Age (c. 1650\u0026ndash;1350 BCE), and \u0026ldquo;Villaggio Grande\u0026rdquo; (\u0026lsquo;Large Village\u0026rsquo;; therein: VG), which developed in the later phases of the Middle Bronze Age and in the Recent Bronze Age (Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e). Continuous habitation persisted in the VG until the later phases of the Late Bronze Age (Bernab\u0026ograve; Brea et al., \u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e1997\u003c/span\u003e; Bernab\u0026ograve; Brea \u0026amp; Cremaschi, \u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e2004\u003c/span\u003e). The moat separating the VP from the VG is 4m deep and it is part of the complex system of hydraulic structures of the site that has been extensively explored (Cremaschi \u0026amp; Pizzi, \u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e2011\u003c/span\u003e, \u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). The metallurgical evidence presented in this paper was recovered from the Recent Bronze Age phases of the VG.\u003c/p\u003e"},{"header":"Materials and methods","content":"\u003cp\u003eSeveral dozens of Bronze Age metallurgical items were recovered at TSRP, including artefacts, crucible fragments and slags (Bianchi, \u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e2018\u003c/span\u003e; Pizzi, \u003cspan citationid=\"CR47\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). In this study, we consider 11 specimens coming from the VG area and selected for in-depth analysis: 5 crucible fragments (two of which from the same fragment 115, see Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e), 1 slag (crucible\u0026rsquo;s slagged surface), and 5 secondary metal by-products (Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e). These specimens were chosen for their representativeness in investigating technical metallurgical processes and their suitability for analysis. Selection criteria included dimensions and structural integrity, as overly brittle specimens were avoided to ensure they withstood the preparation process. To preserve archaeological materials, only fragmented crucibles were considered, and microsamples were extracted from them. The analyses were carried out at the British Museum Department of Scientific Research, using a combination of Digital Microscopy and Scanning Electron Microscopy coupled with Energy Dispersive Spectrometry (SEM-EDS). Following macroscopic investigation, the samples were cut to obtain flat cross-sections using a wet steel bench saw. Then specimens were cold mounted in epoxy resin and the surfaces ground using increasingly finer abrasives and polished down to 1/4\u0026micro; using diamond paste. Reflected Light Microscopy observations were carried out using the Keyence VHX 5000 microscope. Following carbon coating of the samples, SEM-EDS analyses were carried out at high vacuum using a Hitachi S-3700 Scanning Electron Microscope equipped with an Oxford Inc. EDS. An accelerating voltage of 20 kV was used, with a working distance of 10 to 12 mm and a live time of 90 seconds. To optimise quantitative analyses a cobalt standard was used. The analyses were acquired with the Aztec 5.1 software using standard calibrations.\u003c/p\u003e \u003cp\u003eCrucible samples were investigated following the methodology employed by Rademakers and Rehren (\u003cspan citationid=\"CR52\" class=\"CitationRef\"\u003e2016\u003c/span\u003e) and Rademakers et al. (\u003cspan citationid=\"CR53\" class=\"CitationRef\"\u003e2018\u003c/span\u003e). The outer ceramic and the inner vitrified zones were compared. The methodology consists of the analysis of 5 different areas for each zone. The area analysed is the visible area at 100x magnification (\u0026plusmn;\u0026thinsp;1mm\u003csup\u003e2\u003c/sup\u003e). Data analysis and visualization were carried out using R version 4.0.3 (R Core Team, \u003cspan citationid=\"CR49\" class=\"CitationRef\"\u003e2020\u003c/span\u003e) and the \u003cem\u003eggplot2\u003c/em\u003e package (Wickham, \u003cspan citationid=\"CR60\" class=\"CitationRef\"\u003e2016\u003c/span\u003e).\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab1\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 1\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eList of the samples investigated in this study. \u0026ldquo;VG\u0026rdquo; stands for Villaggio Grande.\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"7\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c6\" colnum=\"6\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c7\" colnum=\"7\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eFind ID\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eType\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eSU\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eYear\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c5\"\u003e \u003cp\u003eLocation\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c6\"\u003e \u003cp\u003eOM\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c7\"\u003e \u003cp\u003eSEM-EDS\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e91\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eCrucible\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e2932\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e2002\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eVG\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e124\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eCrucible\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e2518\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e2002\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eVG\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e115a\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eCrucible\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e2790\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e2001\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eVG\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e115b\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eCrucible\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e2790\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e2001\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eVG\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e91a\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eCrucible (only slagged surface)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e2614\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e2001\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eVG\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e149\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eCrucible and bronze\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e2960\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e2002\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eVG\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e19\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eIngot\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e3107\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e2004\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eVG\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e46\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eIngot\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e2379\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e2000\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eVG\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e12\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eCopper\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e8038\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e2010\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eDitch VG (south)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e20\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eBronze\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e1049\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e1999\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eVG\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e104\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eBronze scrap laminae\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e2430\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e2000\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eVG\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003eX\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e"},{"header":"Results","content":"\u003cp\u003eThis section presents the most relevant analytical results, while full results are reported in the Supplementary Materials. The initial part of this section concentrates on the crucible fragments, while the subsequent part focuses on the secondary metallurgical products and by-products. As general consideration, the reader must be aware that most of the considered items show evidence of external weathering in waterlogged conditions. In fact, the whole archaeological site is subject to the fluctuation of the water table and, in some parts, the archaeological sediments were at least seasonally in the saturation zone.\u003c/p\u003e\n\u003ch3\u003eCrucible remains\u003c/h3\u003e\n\u003cp\u003eCrucible fragments measure between 2 and 4 cm in length, with wall thicknesses ranging from 1 to 2.5 cm. Unfortunately, their small dimensions make it impossible to gather information for reconstructing their original size and shape and, in some cases, distinguish between their inner and outer sides. The samples display a predominantly fine, light-coloured fine matrix with a smooth texture. No fiber-like impressions or elongated fractures and porosity, which could indicate the use of organic temper in the fabric, were identified. Additionally, only minimal millimetric inclusions were observed. All the three commonly identified zones in a crucible wall - externally, a fired ceramic zone; centrally, a bloated zone; and internally, a vitrified \u0026lsquo;crucible slag\u0026rsquo; zone (Rademakers et al., \u003cspan class=\"CitationRef\"\u003e2018\u003c/span\u003ea) - were observed, typical for internally heated crucibles. The crucible interiors exhibit variable vitrification or thermal alteration marks, with layers characterized by bloated and slagged green, grey, and black bubbles, displaying increasing porosity towards the crucible interior, exposed to heat at the interface with the crucible charge (Fig. 2). This vitrification is the result of ceramic melting under high heat exposure and fuel ash contamination. A vast range of metal prills and metal oxide inclusions with various compositions were identified in this vitrified zone (thus a \u0026lsquo;crucible slag\u0026rsquo;) for all samples (see \u0026ldquo;Metal prills\u0026rdquo; section below). All 5 samples show the presence of tin in various forms. It is present in the metallic phase as a constituent of bronze (but not as pure tin metal) or as two different oxides. Tin oxides, identified as \u0026ldquo;highly euhedral rhomboids or as needles\u0026rdquo; (Dungworth, \u003cspan class=\"CitationRef\"\u003e2000\u003c/span\u003e) were primarily found in bloated and vitrified areas, as well as on the exterior surface of the bronze fragment TSRP20. These oxides are mainly found in clusters across the crucible surfaces, often associated with copper phases, and are absent in other regions. Tin was also identified as a compound resembling malayaite (CaSnO(SiO\u003csub\u003e4\u003c/sub\u003e)), likely formed through the interaction of SnO\u003csub\u003e2\u003c/sub\u003e with Ca-rich pyroxenes/lime-rich crucible slag (Fig. \u003cspan class=\"InternalRef\"\u003e3\u003c/span\u003ea-d). In some cases, these malayaite-like compounds have a high concentration of iron (TSRP91a, sp. 38\u0026ndash;39), which might be due to either the co-occurrence of iron-bearing minerals in the surrounding environment or the substitution of tin by iron. In malayaite, Fe\u0026sup2;⁺ or Fe\u0026sup3;⁺ ions may substitute for Sn⁴⁺ in the crystal structure because tin and iron have similar ionic radii (similar substitution of iron by tin occurs in the spinel-like oxidation products frequently encountered in crucible slag, e.g. Rademakers et al. \u003cspan class=\"CitationRef\"\u003e2018\u003c/span\u003e). This substitution can occur if tin is less abundant, and iron is prevalent in the system. The extent of substitution can vary. Unfortunately, these crystals offer no insight into the specifics of the alloying process, as they can form during both melting and re-melting, as well as during alloying operations (cf. Rademakers and Farci \u003cspan class=\"CitationRef\"\u003e2018\u003c/span\u003e, and references therein). No traces of cassiterite were found, making it difficult to determine the specific process used at the site to produce bronze.\u003c/p\u003e\n\u003cp\u003eFigure 2 BSE image showing the cross-section of one of the crucibles investigated in the current research (TSRP 124). It shows the full profile of a crucible fragment with bloated layer on the right (crucible interior) and increasingly less vitrified ceramic toward left (exterior, bottom of the sample).\u003c/p\u003e\n\u003cp\u003eSample TSRP 124 exhibits a noticeable crack on its outer side, filled with metal (Fig. 4). Its wall thickness is about 0.5 cm with the thermally unaltered zone between 1 to 3 millimeters. It appears that the exterior section of the crucible wall is missing from this fragment, with only the internal part being preserved, rather than it representing a complete crucible profile. In some cases, though from later periods, the inner sections of crucibles were lined with additional clay to allow for reuse in subsequent melting processes (e.g. Martin\u0026oacute;n-Torres \u0026amp; Rehren, \u003cspan class=\"CitationRef\"\u003e2014\u003c/span\u003e). These details suggest that this fragment could have been part of such a lining. However, no clear evidence of this practice has yet been reported from the Terramare sites. Alternatively, the exterior ceramic zone of the crucible may have broken off from this particular fragment, leaving only the interior section. It is plausible that the observed crack formed during the heating and melting process, allowing liquid metal to seep into the crack (and possible between the original crucible surface and its secondary lining). However, a definitive assessment remains challenging.\u003c/p\u003e\n\u003cp\u003eIn the ceramic bodies of samples TSRP91 and TSRP124, inclusions of monazite ((Ce,La,Nd,Th)PO\u003csub\u003e4\u003c/sub\u003e), a phosphate mineral rich in light rare earth elements, (LREE), were found (TSRP91, sp. 89, TSRP124, sp. 92). Additionally, another inclusion with high presence of iron and chromium was identified in sample TSRP91 (TSRP91, sp. 181). These minerals reflect the selected ceramic fabric for the crucibles rather than the metallurgical processes conducted therein.\u003c/p\u003e\n\u003cp\u003eBulk chemical composition and changes\u003c/p\u003e\n\u003cp\u003eThis section presents the bulk chemical composition and the observed changes between the crucible ceramic and bloated areas of the investigated crucibles (see Tables in the Supplementary Materials for details). In sample TSRP149, only the bloated areas were preserved. Over these, material primarily composed of bronze and its associated oxide products. This may represent a dross layer formed through oxidation during the casting process (Rademakers et al., \u003cspan class=\"CitationRef\"\u003e2018\u003c/span\u003e: 1659). Additionally, several green-coloured, corroded regions were observed along the edge of the bloated zone and adjacent to the metal, likely caused by post-depositional corrosion.\u003c/p\u003e\n\u003cp\u003eThe main elements detected are SiO\u003csub\u003e2\u003c/sub\u003e, Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e, CaO and FeO. Together, these components make up a total of c. 90% for the ceramic areas and c. 88% for the bloated areas. The data were plotted in ternary diagrams, where three selected oxides were normalised to 100%, excluding other detected elements (Fig.\u0026nbsp;5). In the SiO₂-Al₂O₃-FeO ternary diagram, the measurements cluster together, showing uniformity both in the ceramic and in the bloated compositions. All the measurements cluster on the SiO\u003csub\u003e2\u003c/sub\u003e-Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e axis showing only slight variability between their contents. In contrast, the SiO₂-Al₂O₃-CaO ternary diagram reveals a more dispersed distribution of measurements, indicating greater variability in composition. Specifically, there is a noticeable and consistent depletion of lime in the bloated areas compared to the ceramic regions.\u003c/p\u003e\n\u003cp\u003eAdditionally, copper content shows a significant increase, rising from 0.3 wt% (with a maximum value of 0.4 wt%) in the ceramic areas to 2.1 wt% (with a maximum of 3.5 wt%) in the bloated areas. A slight increase is also observed in the tin content, which rises from 0.2 wt% (with a maximum value of 0.3 wt%) in the ceramic areas to 0.5 wt% (with a maximum value of 0.6 wt%) in the bloated areas (see SM).\u003c/p\u003e\n\u003cp\u003eNo charcoal inclusions were identified in the bloated areas. However, indirect evidence of the firing process can be inferred by comparing the crucible ceramic and bloated areas, focusing specifically on lime, alkali and potash content. The relative changes in ratio of oxides to Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e (in wt%) in the bloated areas with respect to the ceramic were measured following the formula from Freestone and Tite (\u003cspan class=\"CitationRef\"\u003e1986\u003c/span\u003e) and Rademakers et al. (\u003cspan class=\"CitationRef\"\u003e2018\u003c/span\u003ea:1657):\u003c/p\u003e\n\u003cdiv id=\"Equa\" class=\"Equation\"\u003e\n \u003cdiv class=\"mathdisplay\" id=\"FileID_Equa\" name=\"EquationSource\"\u003e$$\\:\\frac{\\varDelta\\:\\text{M}\\text{e}\\text{O}}{\\text{A}\\text{l}₂\\text{O}₃\\:}=\\frac{\\frac{\\text{M}\\text{e}\\text{O}\\text{b}\\text{l}\\text{o}\\text{a}\\text{t}\\text{e}\\text{d}}{\\text{A}\\text{l}₂\\text{O}₃\\text{b}\\text{l}\\text{o}\\text{a}\\text{t}\\text{e}\\text{d}}-\\frac{\\text{M}\\text{e}\\text{O}\\text{c}\\text{e}\\text{r}\\text{a}\\text{m}\\text{i}\\text{c}}{\\text{A}\\text{l}₂\\text{O}₃\\text{c}\\text{e}\\text{r}\\text{a}\\text{m}\\text{i}\\text{c}}}{\\frac{\\text{M}\\text{e}\\text{O}\\text{c}\\text{e}\\text{r}\\text{a}\\text{m}\\text{i}\\text{c}}{\\text{A}\\text{l}₂\\text{O}₃\\text{c}\\text{e}\\text{r}\\text{a}\\text{m}\\text{i}\\text{c}}}$$\u003c/div\u003e\n\u003c/div\u003e\n\u003cp\u003eSince alumina is not usually part of the melting charge, normalising metal oxide to Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e avoids distortion from the presence of metals and inclusions. Although the relative changes are minor overall, the comparison of the ceramic and bloated areas (Fig. \u003cspan class=\"InternalRef\"\u003e6\u003c/span\u003e) shows moderate increases in \u003cem\u003esodium (Na₂O)\u003c/em\u003e across the samples, particularly in samples TSRP115b (+\u0026thinsp;56%) and TSRP115a (+\u0026thinsp;33%). \u003cem\u003eMagnesium (MgO)\u003c/em\u003e exhibits a similar pattern, with increases in TSRP115b (+\u0026thinsp;44%) and TSRP115a (+\u0026thinsp;22%). \u003cem\u003eSilica (SiO₂)\u003c/em\u003e demonstrates a relatively lower but consistent increase across all samples, with the most pronounced enrichment in sample TSRP115b (+\u0026thinsp;24%). In contrast, \u003cem\u003ephosphorus (P₂O\u003c/em\u003e\u003cstrong\u003e₅)\u003c/strong\u003e shows moderate depletion in all samples, with reductions ranging from \u0026minus;\u0026thinsp;50% to -80%. \u003cem\u003ePotash (K₂O)\u003c/em\u003e displays varying behaviour. It shows significant increases in sample TSRP91 (+\u0026thinsp;29%) and TSRP115b (+\u0026thinsp;29%) but remains constant in sample TSRP115a. Lime \u003cem\u003e(CaO)\u003c/em\u003e generally shows a notable decrease in all samples, with the strongest depletion occurring in sample TSRP115b (-74%) and TSRP115a (-42%). I\u003cem\u003eron (FeO)\u003c/em\u003e consistently shows a minor increase across all samples, with notable rises in sample TSRP115b (+\u0026thinsp;22%) and TSRP115a (+\u0026thinsp;20%). Finally, both \u003cem\u003etitanium oxide (TiO₂)\u003c/em\u003e and \u003cem\u003emanganese oxide (MnO)\u003c/em\u003e remain unchanged across all samples, indicating that they are not significantly affected by the bloating process and interaction with the crucible charge. Interestingly, it is worth noting that differences were identified between two cross-sections (TSRP115a and TSRP115b) of the same crucible (see Rademakers and Rehren \u003cspan class=\"CitationRef\"\u003e2016\u003c/span\u003e for similar examples). While the general trends are similar, the magnitude of changes is consistently larger in 115b, with greater enrichment in Na₂O, MgO, SiO₂, and K₂O, and a more significant loss of CaO.\u003c/p\u003e\n\u003cp\u003eOverall, the results show how the metallurgical processes led to significant changes in the composition of the crucibles. There is a clear trend of enrichment in sodium, magnesium, silicon, potassium, and iron oxides, while phosphorus and calcium oxides tend to be depleted. These variations likely reflect differences in firing conditions, such as temperature, atmosphere, or material composition (Rademakers \u0026amp; Rehren, \u003cspan class=\"CitationRef\"\u003e2016\u003c/span\u003e). As already largely stated by a number of authors (Evans \u0026amp; Tylecote, \u003cspan class=\"CitationRef\"\u003e1967\u003c/span\u003e; Misra et al., \u003cspan class=\"CitationRef\"\u003e1993\u003c/span\u003e; Rovira, \u003cspan class=\"CitationRef\"\u003e2007\u003c/span\u003e; Tylecote, \u003cspan class=\"CitationRef\"\u003e1982\u003c/span\u003e; Wood, \u003cspan class=\"CitationRef\"\u003e2009\u003c/span\u003e), most of these changes in ratios are due to the chemical interaction of the ceramic body with fuel ash. While this usually involves significant lime contamination too, different wood species produce different ash compositions, resulting in varying crucible slag compositions. Increases in iron oxide content most likely reflect the partitioning of (minor) iron from the metal melt into the crucible slag.\u003c/p\u003e\n\u003ch3\u003eMetal prills\u003c/h3\u003e\n\u003cp\u003eNumerous prills were identified in each crucible fragment, with 121 analyses conducted in total. All prills are copper-based alloys, and a detailed examination revealed their predominantly spherical shape, indicating their transition to a liquid state during processing. Many prills are heavily corroded, often surrounded by metal oxides. Weathered copper-bearing phases with both spheroidal and lath-like growth morphologies were also identified (see Supplementary Materials for details). The sample TSRP91a contains Cu-Sn prills at various stages of oxidation, distributed throughout the entire cross-section. These features, along with the composition ratios of the matrix, which are similar to those of sample 149, suggest that may have originated from the interaction of melted metal with the crucible surface. Despite these transformations, it is important to recognize that oxidation may also result from fluctuating redox conditions within the crucible during the process.\u003c/p\u003e\n\u003cp\u003eDistinctive prills with elevated tin concentrations were found in the bloated and slagged layers of four samples (TSRP91, TSRP115b, TSRP149, TSRP91a). The tin content ranged from 20.3 wt% (TSRP91, sp. 69) to as high as 94.2 wt% (TSRP91, sp. 67). A summary of the elemental concentrations (Minimum, Maximum, Mean, and Standard Deviation (\u0026sigma;)) across the four samples (91a, 91, 149, 115b) is provided in Table \u003cspan class=\"InternalRef\"\u003e2\u003c/span\u003e. A comprehensive list of high-tin prills measured in each sample is provided in the SM (Table 14). The presence of high-tin prills provides direct evidence of intentional alloying of copper (or recycled bronze), (Crew and Rehren,\u0026nbsp;\u003cspan class=\"CitationRef\"\u003e2002\u003c/span\u003e; Rehren, 2001; Rehren and Pusch, 2012). Traces of iron, nickel, arsenic, antimony, and lead were identified in the majority of the investigated prills, with some prills exhibiting traces of silver. Specifically, iron ranged from 0 to 1.7 wt%, nickel from 0 to 1.0 wt%, arsenic from 0.1 to 0.9 wt% and antimony from 0.5 to 3.0 wt%. Lead concentrations varied between 0 to 5.3 wt%. Interestingly, the metal found in the crack and the prills in crucible TSRP124 are primarily composed of copper, with only small amounts of tin present. Two analyses revealed tin concentrations of 2.2 wt% and 2.3 wt%, while two other analyses showed tin concentrations as low as 0.1 wt%. In addition to this, tin oxides were observed on the superficial inner side of the crucible.\u003c/p\u003e\n\u003cdiv class=\"gridtable\"\u003e\u0026nbsp;\u003ctable id=\"Tab2\" border=\"1\"\u003e\n \u003ccaption language=\"En\"\u003e\n \u003cdiv class=\"CaptionNumber\"\u003eTable 2\u003c/div\u003e\n \u003cdiv class=\"CaptionContent\"\u003e\n \u003cp\u003eSummary of the elemental concentrations (Minimum, Maximum, Mean, and Standard Deviation (\u0026sigma;)) across four different samples (91a, 91, 149, 115b). In brackets the number of analyses undertaken.\u003c/p\u003e\n \u003c/div\u003e\n \u003c/caption\u003e\n \u003ccolgroup cols=\"12\"\u003e\u003c/colgroup\u003e\n \u003cthead\u003e\n \u003ctr\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eSample\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eType\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\u0026nbsp;\u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eFe\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eCo\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eNi\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eCu\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eAs\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eAg\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eSn\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eSb\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003ePb\u003c/p\u003e\n \u003c/th\u003e\n \u003c/tr\u003e\n \u003c/thead\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\" rowspan=\"4\"\u003e\n \u003cp\u003e91a (35)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\" rowspan=\"4\"\u003e\n \u003cp\u003eCrucible\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMin\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e54.9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e20.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMax\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e1.7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e78.6\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e42.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e1.7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.7\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMean\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.50\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.53\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.25\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e64.95\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.23\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.10\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e32.95\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e1.03\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.19\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e\u0026sigma;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.39\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.10\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.22\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e6.93\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.15\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e6.35\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.33\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.12\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\" rowspan=\"4\"\u003e\n \u003cp\u003e91 (11)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\" rowspan=\"4\"\u003e\n \u003cp\u003eCrucible\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMin\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e21.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.1\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMax\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e77.6\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e94.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e4.1\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMean\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.26\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e1.40\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.22\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e60.05\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.26\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e37.35\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e1.05\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.85\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e\u0026sigma;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.10\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.24\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e21.91\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.23\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e20.62\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.69\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e1.14\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\" rowspan=\"4\"\u003e\n \u003cp\u003e149 (2)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\" rowspan=\"4\"\u003e\n \u003cp\u003eCrucible\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMin\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e37.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e43\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.1\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMax\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e56.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e61.7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.1\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMean\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e46.75\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.10\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e52.35\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.75\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.10\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e\u0026sigma;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e13.36\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e13.22\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.35\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\" rowspan=\"4\"\u003e\n \u003cp\u003e115b (23)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\" rowspan=\"4\"\u003e\n \u003cp\u003eCrucible\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMin\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e40.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e22.7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.1\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMax\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e73.9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e52.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e1.9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e5.3\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eMean\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.29\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.20\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e59.43\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.14\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e37.32\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e1.10\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e1.74\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e\u0026sigma;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e0.14\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.11\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e6.82\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.06\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\u0026nbsp;\u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e6.24\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.31\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e1.16\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n \u003c/table\u003e\n\u003c/div\u003e\n\u003ch3\u003eSecondary metallurgical products and by-products\u003c/h3\u003e\n\u003cp\u003eThe 5 samples of secondary products investigated exhibited a variety of distinct characteristics in morphology and composition (Fig. 7). The following sections provide an overview of the key structural and compositional features observed in each sample.\u003c/p\u003e\n\u003cp\u003eTwo samples (TSRP19 and TSRP46) consist of almost completely oxidised copper alloy (Fig. 7a-b). Both specimens contain numerous round and elongated copper sulphide inclusions of varying dimensions scattered across their surfaces (Fig. 8a-b). In sample TSRP19 (Fig. 8a), the Cu/S ratio of the copper sulphide inclusions is highly consistent, averaging c. 79 wt% Cu and 21 wt% S, with a comparable Cu/S ratio in sample TSRP46. Both samples displayed voids and porosities across the surface (Fig. 9), which may be attributed to the release of gases such as oxygen, carbon monoxide, carbon dioxide, and sulphur dioxide during oxidation of sulphide inclusions in the molten state (see Hauptmann et al., \u003cspan class=\"CitationRef\"\u003e2016\u003c/span\u003e).\u003c/p\u003e\n\u003cp\u003eTraces of tin (Sn) were detected in 21 out of 40 analyses for TSRP19, with concentrations ranging from 0.1 wt% to 1.2 wt%, and one outlier measuring 7.2 wt% (SR19, sp. 34 of the SM). In contrast, TSRP46 showed minimal traces of tin, with only 9 out of 25 analyses detecting Sn at levels between 0.1 wt% and 0.2 wt%. Additional trace elements identified in TSRP19 include iron, typically ranging from 0 to 0.9 wt% but up to at 4.9 wt%, zinc, with concentrations between 0 and 2 wt%, while silver ranged from 0 to 0.5 wt%, except for a significant peak at 9.5 wt% (TSRP19, sp. 61). Antimony (0 to 1.7 wt%) and lead (0 to 0.8 wt%) were also present, alongside small traces of arsenic and nickel. TSRP46 displayed similar trace element concentrations, with iron typically ranging from 0 to 1.4 wt% and up to 4.8 wt%, zinc between 0 and 1 wt%, silver from 0 to 0.4 wt%, and lead between 0 and 1.1 wt%. By contrast, only low traces of antimony (a maximum of 0.1 wt%) were detected, while arsenic was identified in the range of 0 to 1.3 wt% and up to 3.1 wt%.\u003c/p\u003e\n\u003cp\u003eBoth samples have few inclusions: one metallic inclusion of lead-bismuth (Pb-Bi) was identified in each sample. Lead and bismuth have low solubility in copper and tin alloys, and they tend to segregate into inclusions during solidification. An inclusion of highly oxidised lead was identified in sample TSRP19.\u003c/p\u003e\n\u003cp\u003eSample TSRP20 is a solid metallic bronze fragment with dendritic, as cast structure (Fig. 7d). It illustrates the typical variation in surface preservation due to corrosion. Two distinct concentric layers can be observed: the outer layer, composed of earth minerals and secondary corrosion products and the inner layer, representing the original surface of the fragment and associated corrosion products, predominantly oxidized copper compounds. The various stages of oxidation of copper and tin compounds observed near the surface reflect the progressive exposure to oxygen in the external environment. The metallic area exhibits expanded regions characterized by a tin bronze composition, revealing a dendritic cored (fern-like) texture characterized by small polygonal grains (\u0026alpha;-phase) surrounded by a solution richer in tin (Fig. 10a-b). These dendritic growths are particularly evident in the crystallisation of solid solutions, mostly arise from two-phase alloys (Scott, \u003cspan class=\"CitationRef\"\u003e2012\u003c/span\u003e). The tin content varies across the sample, ranging from approximately 0-0.5 wt% in the dendrite cores, to about 25 wt% in the interdendritic zones (Fig.\u0026nbsp;10b). Due to the substantial difference between these zones, area analyses of approximately 1 mm\u0026sup2; were conducted to discern the chemical composition of the alloy. These analyses revealed a bronze alloy composition with an approximate composition of 95.8 wt% Cu and 4.2 wt% Sn, similar to the composition of the casting flash analyzed in sample TSRP104 (cf. below). Several inclusions were identified within the sample, including exogenic globules of copper sulphides in the films around the grains (Fig.\u0026nbsp;10b). Lead- and sulphur-rich inclusions were also present, likely from sulphide ore minerals residual to raw copper. Oxygen content suggests that partial oxidation has occurred in these sulphide inclusions. Additionally, endogenic inclusions of tin oxides (SnO₂) were found, distributed in the tin-rich zones surrounding the \u0026alpha;-grains. Their presence, far from the oxidized surface, along with the partial oxidation of the lead compounds, indicates that the metal underwent high-temperature reactions, suggesting that oxygen exposure likely occurred during alloying or casting of this object.\u003c/p\u003e\n\u003cp\u003eClose to the exterior surface, various copper and tin compounds at different stages of oxidation were identified, with oxidized copper showing oxygen contents ranging from 8.9 wt% to 33.3 wt%. Numerous tin oxides were also present (Images 7 and 8). Low traces of iron (up to 0.1 wt%), zinc (up to 0.2 wt%), arsenic (up to 2.7 wt%), antimony (up to 2.6 wt%), silver (up to 0.9 wt%), and lead (up to 3.6 wt%) were detected throughout the sample.\u003c/p\u003e\n\u003cp\u003eSample TSRP12 (Fig.\u0026nbsp;7c) is primarily composed of nearly pure copper, with an average composition of 96.7 wt%, determined through four area analyses (TSRP12, sp. 1, 6, 12, and 19). Scattered across the entire surface several small, mainly round copper sulphide inclusions of varying dimensions were identified, averaging 19 wt% S and 77 wt% Cu (TSRP12, sp. 4, 8, 24\u0026ndash;27, 30). Additionally, voids and porosity ranging from a few to several microns were detected throughout the sample. Cubic cuprite crystals were found crystallized within several of these pores. Numerous cuprite inclusions, along with lead- and sulphur-rich inclusions were also observed scattered throughout the sample, likely remnants of the extractive charge. Traces of iron were identified ranging from 0.1 to 0.8 wt%. Zinc concentrations varied between 0 and 0.5 wt%. Low traces of silver (up to 0.2 wt%) and antimony (up to 0.6 wt%) were detected. Lead was found in concentrations ranging from 0 to 1 wt%.\u003c/p\u003e\n\u003cp\u003eSample TSRP104 is characterized by an amalgamation of flat lamellae, with varying lengths and a thickness range between 100 and 200 \u0026micro;m (Fig. 7e). Although a significant portion of these lamellae exhibited pronounced oxidation and weathering on their outer surfaces, 31 analyses were conducted on the low-oxidized areas of these lamellae (Fig. 11a-b), revealing a relatively uniform composition, with an average of 94.3 wt% copper (Cu) and 5.7 wt% tin (Sn). Copper concentrations ranged from 94.9 wt% to 90.3 wt% (\u0026sigma;\u0026thinsp;=\u0026thinsp;1.3), while tin content varied from 7.4 wt% to 3.1 wt% (\u0026sigma;\u0026thinsp;=\u0026thinsp;1.2). Low traces of iron, nickel, zinc, and silver were identified with concentrations up to 0.1\u0026ndash;0.2 wt%. Arsenic, antimony, and lead showed similar values, with concentrations up to 0.3\u0026ndash;0.4 wt%.\u003c/p\u003e"},{"header":"Discussion","content":"\u003cp\u003eThe analysis of the samples investigated has revealed a variety of activities associated with copper and bronze production at the site of TSRP. These findings provide valuable insights into different stages of bronze-related processes, including copper refining, tin alloying for bronze production, and the recycling of bronze materials. In this section, the data presented in the results section is discussed, focusing on how these processes were carried out and on their broader implications.\u003c/p\u003e\n\u003ch3\u003eCopper refining\u003c/h3\u003e\n\u003cp\u003eThe high concentration of copper sulphide inclusions and the presence of numerous voids and porosities observed in samples TSRP19 and TSRP46 suggest that these specimens likely represent (parts of) copper ingots composed of raw or (partially) refined copper. These features align with those typically found in ancient copper bars and ingots, such as the Late Bronze Age copper oxhide ingots from the Uluburun shipwreck (Hauptmann, \u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e2020\u003c/span\u003e, p. 438; Hauptmann et al., \u003cspan citationid=\"CR37\" class=\"CitationRef\"\u003e2016\u003c/span\u003e, pp. 753\u0026ndash;754). The squared shapes of the fragments (Fig.\u0026nbsp;7a-b and Supplementary Materials) further suggest their classification as ingot (fragments). Such characteristics suggest that the copper ingots were not fully refined and were possibly acquired in this semi-processed state before undergoing additional on-site refinement. This scenario is consistent with ancient metallurgical practices, where ingots with impurities were refined closer to the final point of use or manufacturing (Hauptmann et al., \u003cspan citationid=\"CR38\" class=\"CitationRef\"\u003e2002\u003c/span\u003e). Sample TSRP12 likely represents a later stage in the copper refining \u003cem\u003echa\u0026icirc;ne op\u0026eacute;ratoire\u003c/em\u003e. Its small, predominantly round copper sulphide inclusions, present in lower amounts than in the other samples, are likely remnants which were supposed to be removed. This indicates that TSRP12 may be an incompletely refined copper derived from more copper sulphide-rich ingots. Further along in the metallurgical sequence is the cast bronze fragment TSRP20, which contains even lower amounts of copper sulphide inclusions, possibly indicating that it is a newly cast tin-bronze alloy. These sulphide inclusions, mainly dispersed along the films surrounding the grains, cannot recrystallize during working or annealing and offer valuable insights into the alloy's transition from the cast to the worked state (Scott \u0026amp; Schwab, \u003cspan citationid=\"CR57\" class=\"CitationRef\"\u003e2019\u003c/span\u003e).\u003c/p\u003e \u003cp\u003eThe consistent presence of copper sulphides, lead- and sulphur- inclusions, alongside trace elements such as As, Sb, Ni, Ag, Zn, and Pb in samples TSRP19, TSRP46, TSRP12, and TSRP20, suggests a common origin for the metal, possibly from sulfidic and/or sulfosalt ore deposits. These characteristics likely point to consumption at TSRP of copper resulting from the exploitation of the fahlerz-type deposits in the Alpine area, located about 150 km north, which were heavily mined during the Late Bronze Age. (AAcP, \u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e2018\u003c/span\u003e; Addis, \u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2013\u003c/span\u003e; Artioli et al., \u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e2016\u003c/span\u003e; Canovaro et al., \u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e2019\u003c/span\u003e; Ling et al., \u003cspan citationid=\"CR40\" class=\"CitationRef\"\u003e2019\u003c/span\u003e)\u003c/p\u003e\n\u003ch3\u003eIntentional tin-alloying\u003c/h3\u003e\n\u003cp\u003eThe presence of high-tin prills affords key evidence for intentional tin-alloying (e.g. Crew \u0026amp; Rehren, \u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e2002\u003c/span\u003e; Rademakers and Farci \u003cspan citationid=\"CR51\" class=\"CitationRef\"\u003e2018\u003c/span\u003e, Rademakers et al. \u003cspan citationid=\"CR53\" class=\"CitationRef\"\u003e2018\u003c/span\u003ea). During the bronze alloying process prills rich in tin reflect incomplete mixing products which may remain trapped in the vitrified crucible interior. The detection of high-tin prills in specific crucible regions indicates an incomplete amalgamation of copper and tin, serving as tangible evidence for the active alloying of copper or recycled bronze with a tin component. This phenomenon has been extensively investigated and experimentally confirmed by various researchers (e.g. Rademakers and Farci \u003cspan citationid=\"CR51\" class=\"CitationRef\"\u003e2018\u003c/span\u003e, and references therein). The remelting of existing bronze leads to prills with a tin content either lower or equal to that of the recycled bronze. This is because tin, having a higher affinity to oxygen than copper, tends to be depleted from trapped prills under (mildly to strongly) oxidising conditions (e.g. Dungworth, \u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e2000\u003c/span\u003e; Kearns et al., \u003cspan citationid=\"CR39\" class=\"CitationRef\"\u003e2010\u003c/span\u003e; Rademakers \u0026amp; Rehren, \u003cspan citationid=\"CR52\" class=\"CitationRef\"\u003e2016\u003c/span\u003e). When alloying copper or recycled bronze with tin, prills can exhibit any composition between pure copper and tin. It is important to note that no objects with such high tin content have been identified in the Terramare archaeological record and therefore these high-tin prills cannot indicate recycling. Therefore, in the process of producing a low-tin bronze, these high tin prills represent an intermediate product of the alloying process and their presence trapped in the crucible bloated and slagged surfaces are incidental.\u003c/p\u003e \u003cp\u003eHowever, the absence of tin-rich prills in other examined cross-sections does not preclude the examined crucible's use for active alloying or evidence of recycling. This could be due to prills forming only when a complete reaction did not occur in the analyzed area, or because the distribution of tin during alloying is not uniform across the crucible. This is underscored by the analysis of two cross-sections from the same crucible (TSRP115a and TSRP115b), where only the second section revealed high-tin prills, highlighting the variability of process conditions during crucible alloying (as emphasized by Rademakers and Rehren \u003cspan citationid=\"CR52\" class=\"CitationRef\"\u003e2016\u003c/span\u003e).\u003c/p\u003e \u003cp\u003eThe presence of tin oxides combined with the low tin content in the metal prills trapped inside the crucible wall of sample TSRP124 suggests (at least) two possible scenarios, not necessarily mutually exclusive. One hypothesis is that the crucible was used previously for bronze alloying or melting. In this scenario, tin oxides found in the crucible may be residues from earlier alloying operations, where the tin was oxidized and left behind. The crucible was used previously to deal with Cu-Sn alloys and in its final use, only copper may have been melted in the crucible. Another plausible explanation is that the crucible was used for actively alloying copper and tin to produce bronze and during this process, the crack formed before complete mixing of the metals. As a result, the copper-rich metal that seeped through the crack did not fully mix with the tin in the charge, resulting in the low tin content in the seeped metal. At the same time, the unalloyed tin likely oxidized, forming the tin oxides observed inside the crucible.\u003c/p\u003e \u003cp\u003eUnfortunately, it was not possible to identify the source of tin used at the site, as no residual cassiterite grains were observed in the samples. The prills rich in tin do not provide evidence of the source of tin adopted either in metallic or mineral form (cassiterite, SnO₂). It is known that tin in the Middle Bronze Age (Cremaschi et al., \u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e2018\u003c/span\u003e) Late Bronze Age (Berger et al., \u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e2022\u003c/span\u003e; Powell et al., \u003cspan citationid=\"CR48\" class=\"CitationRef\"\u003e2022\u003c/span\u003e) was traded as ingots, but cassiterite is also common in the Alps, making both sources plausible. Cassiterite introduced into a crucible with copper might be reduced to metallic tin before interacting with the copper (Rademakers and Farci, \u003cspan citationid=\"CR51\" class=\"CitationRef\"\u003e2018\u003c/span\u003e, experiments 17\u0026ndash;18). Indeed, it is impossible to determine whether newly formed tin features originated from metal or ore (such as cassiterite) \u0026ndash; although tin oxide inclusions enriched in elements such as tantalum and niobium are indicative of cassiterite use (see also Figueiredo et al., \u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e2017\u003c/span\u003e; Renzi \u0026amp; Rovira, \u003cspan citationid=\"CR54\" class=\"CitationRef\"\u003e2016\u003c/span\u003e). Several methods could have been employed and the more likely are a) co-melting of metallic copper and tin directly, b) cementing metallic copper with natural tin oxide ore (cassiterite) and c) recycling existing bronze, potentially with the addition of copper or tin metal/ore to control the alloy. Other, less likely methods in this context include: d) the natural alloying of Cu-Sn ore (stannite, Cu\u003csub\u003e2\u003c/sub\u003eFeSnS\u003csub\u003e4\u003c/sub\u003e) and e) the co-smelting of Cu ore (azurite, Cu\u003csub\u003e3\u003c/sub\u003e(CO\u003csub\u003e3\u003c/sub\u003e)\u003csub\u003e2\u003c/sub\u003e(OH)\u003csub\u003e2\u003c/sub\u003e, malachite, Cu\u003csub\u003e2\u003c/sub\u003eCO\u003csub\u003e3\u003c/sub\u003e(OH)\u003csub\u003e2\u003c/sub\u003e) and Sn ore (cassiterite, SnO₂). In case d) a higher amount of iron would be expected in the crucible slag. Similarly, in case e), more residue from the copper ore would be expected, especially given that the ore used appears to be \u003cem\u003efahlerz\u003c/em\u003e, which would result in some \u0026ldquo;smelting slag\u0026rdquo; formation within the crucible (Montes-Landa et al., \u003cspan citationid=\"CR43\" class=\"CitationRef\"\u003e2024\u003c/span\u003e for a more detailed discussion; see F. W. Rademakers \u0026amp; Farci, \u003cspan citationid=\"CR51\" class=\"CitationRef\"\u003e2018\u003c/span\u003e).\u003c/p\u003e \u003cdiv id=\"Sec11\" class=\"Section2\"\u003e \u003ch2\u003eBronze recycling\u003c/h2\u003e \u003cp\u003eThe flat laminae observed in sample TSRP104 can be interpreted as by-products of the casting process, commonly referred to as flashes. They typically accumulate at the parting lines of a bivalve mould, where misalignments or gaps between the mould halves, possibly caused by the metal\u0026rsquo;s weight pushing the valves apart, allow excess material to escape and accumulate requiring post-casting removal. The relatively uniform composition of the laminae, which shows a low-tin copper alloy, makes it plausible that these remnants were deliberately collected from one or more objects made of the same alloy for reuse or recycling in subsequent casting processes. The practices of intentional collection and recycling of bronze materials, including small pieces like these lamellae, were likely driven by the need to minimize waste and maximize the utility of existing materials. This suggests a relatively high value placed on bronze, likely in a context of relatively limited access to raw materials.\u003c/p\u003e \u003cp\u003e \u003cb\u003eBonze production at the Terramara of Poviglio\u003c/b\u003e \u003c/p\u003e \u003cp\u003eOverall, these pieces of evidence provide a more nuanced understanding of both the technological and social aspects of metallurgy in one of the most important areas of the Italian peninsula during the Middle and Recent Bronze Ages. Several stages of the bronze production \u003cem\u003echa\u0026icirc;ne op\u0026eacute;ratoire\u003c/em\u003e have been identified at the site:\u003c/p\u003e \u003cp\u003e \u003cul\u003e \u003cli\u003e \u003cp\u003eRefining of raw copper ingots;\u003c/p\u003e \u003c/li\u003e \u003cli\u003e \u003cp\u003eActive alloying (low-tin bronze production);\u003c/p\u003e \u003c/li\u003e \u003cli\u003e \u003cp\u003eBronze casting (though not directly studied in the current research, many metal objects and moulds found on site attest to this process, see Introduction);\u003c/p\u003e \u003c/li\u003e \u003cli\u003e \u003cp\u003eBronze recycling.\u003c/p\u003e \u003c/li\u003e \u003c/ul\u003e \u003c/p\u003e \u003cp\u003eThese stages indicate that local metallurgists possessed specialised knowledge of copper, tin, and bronze properties, as well as expertise in the sequence needed to transform raw copper ingots into pure copper and eventually bronze.\u003c/p\u003e \u003cp\u003eThe discovery of partially refined copper ingots indicates that metallurgists acquired unfinished raw material, rather than opting for finished copper or bronze ingots ready for casting. It can be noted that refining and alloying could in principle take place during a single metallurgical operation (with the removal of dross prior to casting), and the choice for initial refining reflects a particular technological choice which should be compared to other contemporaneous evidence. It may relate to a preference of \u0026lsquo;testing\u0026rsquo; materials before alloying, perhaps as a response to variations in raw copper composition arriving at settlement sites.\u003c/p\u003e \u003cp\u003eThe acquisition of raw copper and the evidence of tin alloying at the site implies that tin, either in a metallic or mineral form, had to be acquired separately too. Since copper and tin often came from different regions and the site of TSRP is located in a territory devoid of any copper and tin ore deposits, the implication is that metallurgists at the site of TSRP, or intermediaries who facilitated the exchange of raw materials between regions, had to participate in distinct or interconnected medium- and long-distance procurement routes for each metal and manage the acquisition and transportation of raw materials before engaging in the production of bronze.\u003c/p\u003e \u003cp\u003eThis work, through evidence of diverse metallurgical practices carried out at the site, allows to highlight the complex and intricate system of metal production and trade networks within the context of the Bronze Age Terramare culture. Future research should focus on extending this investigation on a larger scale, examining specializations in metal and alloy production at different sites with the aim to explore the variability of specialisations and practices at regional and super-regional scale and provide further insight into the economic and social dynamics of Recent Bronze Age communities and trade networks.\u003c/p\u003e \u003c/div\u003e"},{"header":"Conclusions","content":"\u003cp\u003eThis study has provided a detailed examination of the metallurgical practices at the TSRP during the Middle and Recent Bronze Age, shedding light on the complex and multifaceted processes of copper and bronze production. The findings reveal a series of specialised metallurgical techniques of the bronze production \u003cem\u003echa\u0026icirc;ne op\u0026eacute;ratoire\u003c/em\u003e, including the refining of raw copper ingots, the intentional alloying of copper and tin to produce (low-)tin bronze, and the recycling of bronze materials, each indicative of a high level of technical expertise and specialised metallurgical knowledge. The discovery of partially refined copper ingots suggests that raw copper was acquired in an unfinished state and processed locally, rather than being imported as a fully refined product.\u003c/p\u003e \u003cp\u003eThis, along with evidence of active tin-alloying, implies that tin had to be acquired separately, underscoring the site's reliance on long-distance procurement networks. Given that copper and tin deposits were not locally available, these findings reinforce Poviglio's deep integration into interregional trade systems, facilitating the acquisition and transformation of raw materials into high-quality metal objects. Furthermore, the presence of recycled bronze material reflects the importance of metal as a resource and the metallurgists' commitment to minimizing waste and maximizing the utility of available materials in an environment with limited access to raw materials.\u003c/p\u003e \u003cp\u003eFuture research should extend this investigation to other sites of the Terramare culture to explore regional and super-regional variability in metal production. By examining the technological and socio-economic implications of metallurgical practices at different sites, we can gain deeper insights into the role of the Terramare culture in shaping the trade networks and economic systems of the Middle and Late Bronze Age, as well as their broader social dynamics. Moreover, further analysis of metallurgical by-products, including slag and crucible fragments, will be essential for reconstructing the full spectrum of metalworking practices at these sites.\u003c/p\u003e"},{"header":"Declarations","content":"\u003ch2\u003eAuthor Contribution\u003c/h2\u003e\u003cp\u003eA.A. and F.W.R. conceptualized the study and developed the research framework. A.A. carried out the archaeological sampling and laboratory analyses. A.A. and F.W.R. interpreted the metallurgical data and prepared the data visualizations. A.Z. and M.C. provided the archaeological context and reviewed the relevant archaeological and historical literature. A.A. and A.Z. drafted the main manuscript text. All authors contributed to the interpretation of the results, revised the manuscript, and approved the final version.\u003c/p\u003e\u003ch2\u003eAcknowledgement\u003c/h2\u003e\u003cp\u003eThe archaeological excavation of the Terramara of Santa Rosa di Poviglio is going on since 1984 under the direction of MC and since 2019 of AZ. The Italian Ministry of Culture (MiC) released the permits for archaeological excavation and sampling archaeological materials. We would like to thank the Municipality of Poviglio and the collaborators of the Museo della Terramara for the continuous support. The archaeological investigation at Santa Rosa di Poviglio was supported by the University of Milano (Fondi Speciali per le Ricerche Archeologiche), the Municipality of Poviglio and Coopsette. Additional contribution comes from an action of the National Recovery and Resilience Plan (NRRP): Cultural Heritage Active Innovation for Sustainable Society (CHANGES) Project, funded by the European Union \u0026ndash; NextGenerationEU, under the National Recovery and Resilience Plan (NRRP) Mission 4, Component 2, Investment Line 1.3.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\n\u003cli\u003eAAcP. (2018). \u003cem\u003eAlpine Archaeocopper Project.\u003c/em\u003e [Dataset]. http://www.geoscienze. unipd.it/aacp/welcome.html.\u003c/li\u003e\n\u003cli\u003eAddis, A. (2013). \u003cem\u003eLate Bronze Age metallurgy in the Italian Eastern Alps: Copper smelting slags and mine exploitation\u003c/em\u003e [PhD Thesis]. Universit\u0026agrave; di Trento.\u003c/li\u003e\n\u003cli\u003eAngelini, A., Angelini, I., Artioli, G., Nimis, P., \u0026amp; Villa, I. M. (2015). Tipologia e archeometria dei bronzi di Castel de Pedena (San Gregorio nelle Alpi, Belluno). In G. 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Phase Equilibria at Liquidus Temperatures in the System Iron Oxide\u0026ndash;Al\u003csub\u003e2\u003c/sub\u003e O\u003csub\u003e3\u003c/sub\u003e \u0026ndash;SiO\u003csub\u003e3\u003c/sub\u003e in Air Atmosphere. \u003cem\u003eJournal of the American Ceramic Society\u003c/em\u003e, \u003cem\u003e40\u003c/em\u003e(4), 121\u0026ndash;133. https://doi.org/10.1111/j.1151-2916.1957.tb12588.x\u003c/li\u003e\n\u003cli\u003ePeroni, R. (1994). \u003cem\u003eI pugnali nell\u0026rsquo;Italia continentale.: Vol. VI.10\u003c/em\u003e.\u003c/li\u003e\n\u003cli\u003ePeroni, R., \u0026amp; Carancini, G. L. (1997). La koin\u0026egrave; metallurgica. In M. Bernab\u0026ograve; Brea, A. Cardarelli, \u0026amp; M. Cremaschi (Eds.), \u003cem\u003eLe Terramare. La pi\u0026ugrave; antica civilt\u0026agrave; padana\u003c/em\u003e (pp. 595\u0026ndash;601). Electa.\u003c/li\u003e\n\u003cli\u003ePizzi, C. (2021). I materiali in Bronzo. In M. Cremaschi \u0026amp; C. 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Bronze metallurgy in the Late Phrygian settlement of Gordion, Turkey. \u003cem\u003eArchaeological and Anthropological Sciences\u003c/em\u003e, \u003cem\u003e10\u003c/em\u003e(7), Article 7. https://doi.org/10.1007/s12520-017-0475-8.\u003c/li\u003e\n\u003cli\u003eRenzi, M., \u0026amp; Rovira, S. (2016). Metallurgical vessels from the Phoenician site of La Fonteta (Alicante, Spain): A typological and analytical study. In G. K\u0026ouml;rlin, M. Prange, T. St\u0026ouml;llner, \u0026amp; Yal\u0026ccedil;in, U. (Eds.), \u003cem\u003eFrom Bright Ores to Shiny Metals. Festschrift for Andreas Hauptmann on the Occasion of 40 Years Research in Archaeometallurgy and Archaeometry\u003c/em\u003e (pp. 143\u0026ndash;146). https://discovery.ucl.ac.uk/id/eprint/10039567/\u003c/li\u003e\n\u003cli\u003eRovira, S. (2007). La producci\u0026oacute;n de bronces en la Prehistoria. In J. Molera, J. Farjas, P. Roura, \u0026amp; T. Pradell (Eds.), \u003cem\u003eAvances en Arqueometr\u0026iacute;a. \u003c/em\u003e\u003cem\u003eActas Del VI Congreso Ib\u0026eacute;rico De Arqueometr\u0026iacute;a 2005\u003c/em\u003e (pp. 21\u0026ndash;35).\u003c/li\u003e\n\u003cli\u003eScott, D. A. (2012). \u003cem\u003eAncient metals: Microstructure and metallurgy. Volume I: Vol. I. Copper and copper alloys\u003c/em\u003e. CSP: Conservation Science Press.\u003c/li\u003e\n\u003cli\u003eScott, D. A., \u0026amp; Schwab, R. (2019). \u003cem\u003eMetallography in Archaeology and Art\u003c/em\u003e. Springer International Publishing.\u003c/li\u003e\n\u003cli\u003eTylecote, R. F. (1982). The Late Bronze Age: Copper and bronze metallurgy at Enkomi and Kition. In J. D. Muhly, R. Maddin, \u0026amp; V. Karageorghis (Eds.), \u003cem\u003eEarly Metallurgy in Cyprus, 4000\u0026ndash; 500 BC\u003c/em\u003e (pp. 81\u0026ndash;100). Pierides Foundation.\u003c/li\u003e\n\u003cli\u003eVicenzutto, D., Dalla Longa, E., Angelini, I., Artioli, G., Nimis, P., \u0026amp; Villa, I. M. (2015). Manufatti in bronzo del sito arginato di Fondo Paviani (Verona)\u0026ndash;Scavi Universit\u0026agrave; di Padova 2007\u0026ndash;2012. Inquadramento tipocronologico e analisi archeometriche. \u003cem\u003eStudi Di Preistoria e Protostoria\u0026mdash;2\u0026mdash;Preistoria e Protostoria Del Veneto.\u003c/em\u003e, 833\u0026ndash;838.\u003c/li\u003e\n\u003cli\u003eWickham, H. (2016). \u003cem\u003eggplot2: Elegant graphics for data analysis\u003c/em\u003e. springer.\u003c/li\u003e\n\u003cli\u003eWood, N. (2009). Some implications of the use of wood ash in Chinese stoneware glazes. In A. Shortland, I. C. Freestone, \u0026amp; T. Rehren (Eds.), \u003cem\u003eFrom Mine to Microscope. Advances in the Study of Ancient Technology\u003c/em\u003e (pp. 51\u0026ndash;60). Oxbow Books.\u003c/li\u003e\n\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":false,"highlight":"","institution":"","isAcceptedByJournal":true,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"archaeological-and-anthropological-sciences","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"aasc","sideBox":"Learn more about [Archaeological and Anthropological Sciences](http://link.springer.com/journal/12517)","snPcode":"12520","submissionUrl":"https://submission.nature.com/new-submission/12520/3","title":"Archaeological and Anthropological Sciences","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false},"keywords":"Terramare culture, Bronze Age metallurgy, Chaîne opératoire, SEM-EDS","lastPublishedDoi":"10.21203/rs.3.rs-6572450/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-6572450/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eDuring the Middle and Recent Bronze Age (c. 1350\u0026ndash;1150/1100 BCE), the Terramare culture played a crucial role in the development of both regional and interregional trade networks of the Po Plain of northern Italy, particularly through the production and exchange of metal artefacts. While substantial research has focused on the bronze objects themselves, the technical aspects of metal production, such as refining, alloying and recycling methods, remain underexplored. This study addresses this gap by analyzing a series of metallurgical by-products from the Terramara Santa Rosa di Poviglio site, including crucible fragments, and secondary metal remains. Utilizing Digital Microscopy and Scanning Electron Microscopy combined with Energy Dispersive Spectroscopy (SEM-EDS), we investigate the technical practices involved in copper and bronze production at the site. The results indicate the local processing of partially refined copper ingots, intentional alloying of copper and tin, and the recycling of bronze, demonstrating specialised metallurgical expertise. Moreover, these findings suggest that Santa Rosa di Poviglio was deeply integrated into long-distance trade networks, acquiring raw copper and tin for alloying and production of high-quality metal objects. Overall, this research enhances our understanding of Middle Recent Bronze Age metalworking practices and the socio-economic dynamics of the Terramare culture, paving the way for further studies on metallurgical techniques at other Bronze Age sites of the area to explore regional variations and broader economic connections.\u003c/p\u003e","manuscriptTitle":"Decoding bronze production at Terramara Santa Rosa di Poviglio site (Bronze Age, N Italy): Insights from secondary production waste","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-05-11 10:20:03","doi":"10.21203/rs.3.rs-6572450/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Revision requested","date":"2025-09-10T15:29:03+00:00","index":"","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2025-05-26T19:03:53+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2025-05-21T14:19:16+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2025-05-20T16:03:54+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"338002748911646885505073661567113944835","date":"2025-05-06T21:45:31+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"59524830812237690485252589589782857800","date":"2025-05-06T18:23:30+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"19883156064188484255525508133260047547","date":"2025-05-06T17:59:02+00:00","index":"hide","fulltext":""},{"type":"reviewersInvited","content":"","date":"2025-05-06T17:20:37+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2025-05-02T07:09:44+00:00","index":"","fulltext":""},{"type":"checksComplete","content":"","date":"2025-05-02T05:48:57+00:00","index":"","fulltext":""},{"type":"submitted","content":"Archaeological and Anthropological Sciences","date":"2025-05-01T14:09:55+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"archaeological-and-anthropological-sciences","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"aasc","sideBox":"Learn more about [Archaeological and Anthropological Sciences](http://link.springer.com/journal/12517)","snPcode":"12520","submissionUrl":"https://submission.nature.com/new-submission/12520/3","title":"Archaeological and Anthropological Sciences","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false}}],"origin":"","ownerIdentity":"106a8b6f-87f1-4033-a36b-886b1ac828e2","owner":[],"postedDate":"May 11th, 2025","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"published-in-journal","subjectAreas":[],"tags":[],"updatedAt":"2025-12-08T15:58:46+00:00","versionOfRecord":{"articleIdentity":"rs-6572450","link":"https://doi.org/10.1007/s12520-025-02357-6","journal":{"identity":"archaeological-and-anthropological-sciences","isVorOnly":false,"title":"Archaeological and Anthropological Sciences"},"publishedOn":"2025-12-05 15:56:55","publishedOnDateReadable":"December 5th, 2025"},"versionCreatedAt":"2025-05-11 10:20:03","video":"","vorDoi":"10.1007/s12520-025-02357-6","vorDoiUrl":"https://doi.org/10.1007/s12520-025-02357-6","workflowStages":[]},"version":"v1","identity":"rs-6572450","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-6572450","identity":"rs-6572450","version":["v1"]},"buildId":"8U1c8b4HqxoKbykW_rLl7","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}