This work presents an evaluation of various methods for in situ high‐precision Sr and Pb isotopic determination in archaeological glass (containing 100–500 μg g−1 target element) by nanosecond laser ablation multi‐collector‐inductively coupled plasma‐mass spectrometry (ns‐LA‐MC‐ICP‐MS). A set of four soda‐lime silicate glasses, Corning A–D, mimicking the composition of archaeological glass and produced by the Corning Museum of Glass (Corning, New York, USA), were investigated as candidates for matrix‐matched reference materials for use in the analysis of archaeological glass. Common geological reference materials with known isotopic compositions (USGS basalt glasses BHVO‐2G, GSE‐1G and NKT‐1G, soda‐lime silicate glass NIST SRM 610 and several archaeological glass samples with known Sr isotopic composition) were used to evaluate the ns‐LA‐MC‐ICP‐MS analytical procedures. When available, ns‐LA‐MC‐ICP‐MS results for the Corning glasses are reported. These were found to be in good agreement with results obtained via pneumatic nebulisation (pn) MC‐ICP‐MS after digestion of the glass matrix and target element isolation. The presence of potential spectral interference from doubly charged rare earth element (REE) ions affecting Sr isotopic determination was investigated by admixing Er and Yb aerosols by means of pneumatic nebulisation into the gas flow from the laser ablation system. It was shown that doubly charged REE ions affect the Sr isotope ratios, but that this could be circumvented by operating the instrument at higher mass resolution. Multiple strategies to correct for instrumental mass discrimination in ns‐LA‐MC‐ICP‐MS and the effects of relevant interferences were evaluated. Application of common glass reference materials with basaltic matrices for correction of ns‐LA‐MC‐ICP‐MS isotope data of archaeological glasses results in inaccurate Pb isotope ratios, rendering application of matrix‐matched reference materials indispensable. Correction for instrumental mass discrimination using the exponential law, with the application of Tl as an internal isotopic standard element introduced by pneumatic nebulisation and Corning D as bracketing isotopic calibrator, provided the most accurate results for Pb isotope ratio measurements in archaeological glass. Mass bias correction relying on the power law, combined with intra‐element internal correction, assuming a constant 88Sr/86Sr ratio, yielded the most accurate results for 87Sr/86Sr determination in archaeological glasses
Sb was frequently used as a raw material, both in ancient glass-making (as an opacifier and decolouriser) and metallurgy (either as an alloying element or as a pure metal). Despite this ubiquity, antimony production has only occasionally been studied and questions concerning its provenance are still not satisfactorily answered. This study evaluates the suitability of Sb isotope analysis for provenance determination purposes, as experiments under lab conditions have revealed fractionation occurring during redox processes in oxidising stibnites and in making opacified glasses. The results of this paper help to evaluate the possible influence of the pyrotechnological processes on the antimony isotope composition of glass artefacts. This paper focuses on the Caucasus as case study by applying mineralogical, geochemical and isotopic analysis to Georgian ores (mainly from the Racha-Lechkumi district) and Late Bronze Age (LBA; 15th-10th century BCE) metallic Sb objects found at the sites of Brili and Chalpiragorebi.
In large parts of the Mediterranean recipes for the earliest man-made glass changed from melting mixtures of crushed quartz pebbles and halophytic plant ashes in the Late Bronze Age to the use of quartz sands and mineral soda during the Early Iron Age. Not much is known about this transition and the experimental materials which would inevitably have been connected to such technological change. In this paper we present a unique snapshot of developments in glass technology in Anatolia during the Middle Iron Age, when glass is still a relatively rare commodity. The present work focusses on black glass beads decorated with yellow trails from eighth to seventh century BCE Sardis, glass beads that are very rare for this period, and on this site. A full elemental analysis of the beads was made, and Sr, Pb and B isotope ratios were determined. This study reveals the use of a combination of a previously unknown source of silica and of mineral soda, giving rise to elevated (granite-like) Sr isotope signatures, as well as high alumina and B concentrations. The yellow trails of glass on the beads consist of leadtin yellow type II, lead stannate, showing the earliest occurrence of this type of opacifier/colourant so far, predating any other findings by at least four centuries. The production of these glass beads may be local to Sardis and experimental in nature. It is therefore suggested that Sardis may have played its role in the technological development of the glass craft during the Iron Age.
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