Roman coloured glass in the Western provinces: The glass cakes and tesserae from West Clacton in England

In this study, we introduce a Hewlett-Packard prototype picoliter pipette, the “thermal inkjet picofluidic system” (TIPS), for analytical purposes. In contrast to the use of actual inkjet printers, this instrument allows for control of all energy and time settings. We are able to show that in contrast to techniques delivering microliter and nanoliter volumes, evaporation has a major influence on the deposition of picoliter volumes and has to be treated seriously when picoliter depositions are applied in the laboratory for calibration purposes. We developed a strategy to reduce evaporation by varying different parameters, thereby achieving a precision of less than 10% for elemental depositions ranging from 1 to 300 picoliters and 1 to 2000 pg elemental deposits. Additionally, we determined the performance of the micro X-ray fluorescence (MXRF) instruments in terms of limit of detection (LODs), focal spot size, sensitivity, and precision and evaluated the TIPS deposits as reference materials for MXRF using ...

Picoliter droplet deposition using a prototype picoliter pipette: control parameters and application in micro X-ray fluorescence.

A set of Roman glass fragments, excavated at Sevilla and dated in the 5th century A.D., has been analysed by PIXE and PIGE techniques using the external beam set-up of the 3 MV tandem Pelletron accelerator of the CNA at the University of Sevilla. Using a simple quantification method, based on the indirect charge calculation on the sample by monitoring the X-ray induced by the proton beam on the exit window, the composition of the glasses has been determined. From the obtained results, the use of soda as flux has been inferred and colouring manufacture procedures have been identified.

PIXE–PIGE analysis of late roman glass fragments

Twenty-six tesserae (red, orange, yellow, light amber, green, blue and white) from the balneum of the villa at Faragola (Ascoli Satriano, Foggia) have been examined by colorimetry, ICP–MS, ICP–OES and SEM–EDS. Different types of calcareous sands have been used as the source of silica (network former), also providing the stabilizing agent. A natron-type soda source served as the network modifier; however, the use of a sodium-rich plant ash and the recycling process have been hypothesized for the production of two tesserae (FT 1 red and FT 3 orange). The colouring and opacifying agents were Cu oxide (cuprite, orange), metallic copper (red), Pb antimonates (yellow), Ca antimonates (white), a mixture of copper (Cu2+) and Pb antimonates (green), a mixture of cobalt (Co2+) or copper (Cu2+) and Ca antimonates (blue). The light amber tesserae should owe their colour to iron (Fe3+) alone or associated with sulphide (S2−) and Ca antimonates. It is likely that the Faragola tesserae were locally produced in a secondary glass workshop.

The coloured tesserae decorating the vaults of the faragola balneum (ascoli satriano, foggia, southern italy)

Float glass-type SiO2-Na2O-CaO glasses with 0 – 10 mol% Sb2O3 were melted and their compositional, structural, thermal and optical properties characterised. All glasses were X-ray amorphous and increasing Sb2O3 content progressively decreased glass transition temperature (Tg) and dilatometric softening point (Td), despite increases in Al2O3 content from greater crucible corrosion. 121Sb Mossbauer spectroscopy confirmed that Sb was predominantly incorporated as Sb3+ (Sb3+/ΣSb ~ 0.9) and Raman spectroscopy showed that Sb substantially decreased average (Si, Al)-O Qn speciation. Both techniques confirmed that Sb3+ ions were incorporated in trigonal pyramidal [:SbO3] polyhedra. XRF and Raman spectroscopies confirmed that SO3 content decreased with increasing Sb2O3 content. TGA analysis showed, as a linear function of Sb2O3 content, mass gain commencing at 700°C, reaching a maximum at 1175°C, then mass loss above 1175°C, consistent with oxidation (Sb3+ → Sb5+) then reduction (Sb5+ → Sb3+). The TGA samples were shown to have attained or approached Sb redox equilibrium during measurement. Optical absorption spectroscopy (UV-Vis-nIR) showed red-shifts of the UV absorption edge with increasing Sb2O3 content, consistent with increasing intensity of far-UV absorption bands from Sb3+ and Sb5+ s→p transitions. UV-Vis-nIR fluorescence spectroscopy evidenced a broad luminescence band centred at ~25,000 cm−1, attributed to the 3P1→1S0 transition of Sb3+, which is Stokes shifted by ~15,000 cm−1 from the 1S0→3P1 absorption at ~40,000 cm−1. The most intense emission occurred at 0.5 mol% Sb2O3, with concentration quenching reducing luminescence intensities at higher Sb2O3 contents. Additions of Sb2O3 to float-type soda-lime-silica glasses could thus enable lower melting energies and/or new solar energy applications.

/pdf/composition-structure-property-effects-of-antimony-in-soda-3f97leeak5.pdf

Composition-structure-property effects of antimony in soda-lime-silica glasses

A set of Roman glass fragments, excavated at Bliesbruck–Reinheim (French–German border), were analysed by electron probe microanalysis (EPMA) and micro-synchrotron radiation-induced x-ray fluorescence (m-SRXRF) in order to determine the major, minor and trace chemical composition. Based on this analysis, five classes of mono-coloured glass could be discerned. However, one piece of this set was not mono-coloured, but consisted of a mixture of brown and white opaque glass. This fragment was investigated using EPMA and transmission electron microscopy (TEM) in order to gain a better insight into its microstructure. Both colours proved to contain small crystalline inhomogeneities. Structural information reveals the form in which the detected elements are present and helps to explain the appearance (e.g. colour) of the material. Copyright  2004 John Wiley & Sons, Ltd.

http://ematweb.cmi.ua.ac.be/emat/pdf/1246.pdf

EPMA and µ‐SRXRF analysis and TEM‐based microstructure characterization of a set of Roman glass fragments

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EPMA and µ‐SRXRF analysis and TEM‐based microstructure characterization of a set of Roman glass fragments