Unravelling the role of iron and manganese oxides in colouring Late Antique glass by micro-XANES and micro-XRF spectroscopies
This research aims to understand colouring technologies in 5th–7th centuries glass imported to Atlantic Britain by correlating the iron (Fe) and manganese (Mn) ratios and oxidation states with colour. Despite having a similar matrix chemical composition and concentrations of Fe and Mn oxides, these...
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| Published in: | JPhys photonics Vol. 6; no. 2; pp. 25001 - 25019 |
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| Main Authors: | , , , , , |
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| Language: | English |
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01.04.2024
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| ISSN: | 2515-7647, 2515-7647 |
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| Abstract | This research aims to understand colouring technologies in 5th–7th centuries glass imported to Atlantic Britain by correlating the iron (Fe) and manganese (Mn) ratios and oxidation states with colour. Despite having a similar matrix chemical composition and concentrations of Fe and Mn oxides, these vessels display different colours (from green to yellow/amber, sometimes with purple streaks). Colour changes can be induced by controlling the reduction-oxidation reactions that occur during glass production, which are influenced by the raw materials, furnace and melt atmosphere, and recycling. To evaluate these parameters, reference glasses were prepared, following the composition of Late Antique archaeological glass recovered from Tintagel (UK) and Whithorn (UK). A corpus of archaeological and experimental glass samples was analysed using bulk Fe and Mn K-edge x-ray absorption near edge structure (XANES) spectroscopy, micro-XANES and micro x-ray fluorescence (
μ
-XRF) at beamline ID21, at the European Synchrotron Radiation Facility. Fe and Mn XANES spectra of the archaeological glass indicate that Fe and Mn are in a similar oxidation state in all the yellow samples, predominantly Fe
3+
and Mn
2+
. No detectable difference in Mn and Fe oxidation state occurs in the purple streaks compared to the yellow glass bulk but
μ
-XRF maps of the distribution of Fe and Mn show that Mn is more concentrated in the purple streaks. This indicates that the purple colour of the streaks is mainly due to a higher Mn/Fe ratio and persistence of more oxidised manganese in the purple areas, even though it is difficult to detect. Many archaeological fragments appear pale green in transmitted light but amber in reflected light. XANES studies detected the presence of surface layers where manganese is more oxidised. This layer is believed to scatter transmitted and reflected light differently and might be responsible for the optical features of the archaeological glass. |
|---|---|
| AbstractList | Abstract This research aims to understand colouring technologies in 5th–7th centuries glass imported to Atlantic Britain by correlating the iron (Fe) and manganese (Mn) ratios and oxidation states with colour. Despite having a similar matrix chemical composition and concentrations of Fe and Mn oxides, these vessels display different colours (from green to yellow/amber, sometimes with purple streaks). Colour changes can be induced by controlling the reduction-oxidation reactions that occur during glass production, which are influenced by the raw materials, furnace and melt atmosphere, and recycling. To evaluate these parameters, reference glasses were prepared, following the composition of Late Antique archaeological glass recovered from Tintagel (UK) and Whithorn (UK). A corpus of archaeological and experimental glass samples was analysed using bulk Fe and Mn K-edge x-ray absorption near edge structure (XANES) spectroscopy, micro-XANES and micro x-ray fluorescence ( μ -XRF) at beamline ID21, at the European Synchrotron Radiation Facility. Fe and Mn XANES spectra of the archaeological glass indicate that Fe and Mn are in a similar oxidation state in all the yellow samples, predominantly Fe 3+ and Mn 2+ . No detectable difference in Mn and Fe oxidation state occurs in the purple streaks compared to the yellow glass bulk but μ -XRF maps of the distribution of Fe and Mn show that Mn is more concentrated in the purple streaks. This indicates that the purple colour of the streaks is mainly due to a higher Mn/Fe ratio and persistence of more oxidised manganese in the purple areas, even though it is difficult to detect. Many archaeological fragments appear pale green in transmitted light but amber in reflected light. XANES studies detected the presence of surface layers where manganese is more oxidised. This layer is believed to scatter transmitted and reflected light differently and might be responsible for the optical features of the archaeological glass. This research aims to understand colouring technologies in 5th–7th centuries glass imported to Atlantic Britain by correlating the iron (Fe) and manganese (Mn) ratios and oxidation states with colour. Despite having a similar matrix chemical composition and concentrations of Fe and Mn oxides, these vessels display different colours (from green to yellow/amber, sometimes with purple streaks). Colour changes can be induced by controlling the reduction-oxidation reactions that occur during glass production, which are influenced by the raw materials, furnace and melt atmosphere, and recycling. To evaluate these parameters, reference glasses were prepared, following the composition of Late Antique archaeological glass recovered from Tintagel (UK) and Whithorn (UK). A corpus of archaeological and experimental glass samples was analysed using bulk Fe and Mn K-edge x-ray absorption near edge structure (XANES) spectroscopy, micro-XANES and micro x-ray fluorescence ( μ -XRF) at beamline ID21, at the European Synchrotron Radiation Facility. Fe and Mn XANES spectra of the archaeological glass indicate that Fe and Mn are in a similar oxidation state in all the yellow samples, predominantly Fe ^3+ and Mn ^2+ . No detectable difference in Mn and Fe oxidation state occurs in the purple streaks compared to the yellow glass bulk but μ -XRF maps of the distribution of Fe and Mn show that Mn is more concentrated in the purple streaks. This indicates that the purple colour of the streaks is mainly due to a higher Mn/Fe ratio and persistence of more oxidised manganese in the purple areas, even though it is difficult to detect. Many archaeological fragments appear pale green in transmitted light but amber in reflected light. XANES studies detected the presence of surface layers where manganese is more oxidised. This layer is believed to scatter transmitted and reflected light differently and might be responsible for the optical features of the archaeological glass. This research aims to understand colouring technologies in 5th–7th centuries glass imported to Atlantic Britain by correlating the iron (Fe) and manganese (Mn) ratios and oxidation states with colour. Despite having a similar matrix chemical composition and concentrations of Fe and Mn oxides, these vessels display different colours (from green to yellow/amber, sometimes with purple streaks). Colour changes can be induced by controlling the reduction-oxidation reactions that occur during glass production, which are influenced by the raw materials, furnace and melt atmosphere, and recycling. To evaluate these parameters, reference glasses were prepared, following the composition of Late Antique archaeological glass recovered from Tintagel (UK) and Whithorn (UK). A corpus of archaeological and experimental glass samples was analysed using bulk Fe and Mn K-edge x-ray absorption near edge structure (XANES) spectroscopy, micro-XANES and micro x-ray fluorescence ( μ -XRF) at beamline ID21, at the European Synchrotron Radiation Facility. Fe and Mn XANES spectra of the archaeological glass indicate that Fe and Mn are in a similar oxidation state in all the yellow samples, predominantly Fe 3+ and Mn 2+ . No detectable difference in Mn and Fe oxidation state occurs in the purple streaks compared to the yellow glass bulk but μ -XRF maps of the distribution of Fe and Mn show that Mn is more concentrated in the purple streaks. This indicates that the purple colour of the streaks is mainly due to a higher Mn/Fe ratio and persistence of more oxidised manganese in the purple areas, even though it is difficult to detect. Many archaeological fragments appear pale green in transmitted light but amber in reflected light. XANES studies detected the presence of surface layers where manganese is more oxidised. This layer is believed to scatter transmitted and reflected light differently and might be responsible for the optical features of the archaeological glass. This research aims to understand colouring technologies in 5th–7th centuries glass imported to Atlantic Britain by correlating the iron (Fe) and manganese (Mn) ratios and oxidation states with colour. Despite having a similar matrix chemical composition and concentrations of Fe and Mn oxides, these vessels display different colours (from green to yellow/amber, sometimes with purple streaks). Colour changes can be induced by controlling the reduction-oxidation reactions that occur during glass production, which are influenced by the raw materials, furnace and melt atmosphere, and recycling. To evaluate these parameters, reference glasses were prepared, following the composition of Late Antique archaeological glass recovered from Tintagel (UK) and Whithorn (UK). A corpus of archaeological and experimental glass samples was analysed using bulk Fe and Mn K-edge x-ray absorption near edge structure (XANES) spectroscopy, micro-XANES and micro x-ray fluorescence (μ-XRF) at beamline ID21, at the European Synchrotron Radiation Facility. Fe and Mn XANES spectra of the archaeological glass indicate that Fe and Mn are in a similar oxidation state in all the yellow samples, predominantly Fe3+ and Mn2+. No detectable difference in Mn and Fe oxidation state occurs in the purple streaks compared to the yellow glass bulk but μ-XRF maps of the distribution of Fe and Mn show that Mn is more concentrated in the purple streaks. This indicates that the purple colour of the streaks is mainly due to a higher Mn/Fe ratio and persistence of more oxidised manganese in the purple areas, even though it is difficult to detect. Many archaeological fragments appear pale green in transmitted light but amber in reflected light. XANES studies detected the presence of surface layers where manganese is more oxidised. This layer is believed to scatter transmitted and reflected light differently and might be responsible for the optical features of the archaeological glass. |
| Author | Gherardi, Francesca Cotte, Marine Tyson, Rachel Hole, Clément Paynter, Sarah Campbell, Ewan |
| Author_xml | – sequence: 1 givenname: Francesca orcidid: 0000-0003-0469-8154 surname: Gherardi fullname: Gherardi, Francesca organization: Investigative Science, Historic England , Portsmouth, United Kingdom – sequence: 2 givenname: Clément surname: Hole fullname: Hole, Clément organization: European Synchrotron Radiation Facility (ESRF) , Grenoble, France – sequence: 3 givenname: Ewan surname: Campbell fullname: Campbell, Ewan organization: School of Humanities, University of Glasgow , Glasgow, United Kingdom – sequence: 4 givenname: Marine surname: Cotte fullname: Cotte, Marine organization: LAMS, CNRS UMR 8220, Sorbonne Université , UPMC Univ Paris 06, Paris, France – sequence: 5 givenname: Rachel surname: Tyson fullname: Tyson, Rachel organization: Consultant glass specialist , Stroud, United Kingdom – sequence: 6 givenname: Sarah surname: Paynter fullname: Paynter, Sarah organization: Investigative Science, Historic England , Portsmouth, United Kingdom |
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| Cites_doi | 10.1039/C6JA00356G doi:10.1016/j.jasrep.2015.08.009 10.1127/0935-1221/2002/0014-0749 doi:10.1016/j.chemgeo.2005.03.004 10.1111/j.1475-4754.2010.00534.x doi:10.1016/S0022-3093(98)00728-5 doi:10.1016/j.jas.2008.08.008 doi:10.1016/j.jnoncrysol.2022.121710 doi:10.1111/j.1475-4754.2000.tb00887.x 10.2138/am-2001-5-612 10.2138/am.2012.3903 10.1127/0935-1221/2011/0023-2125 doi:10.1016/j.corsci.2018.08.012 10.1088/1742-6596/430/1/012007 10.1179/sic.2008.53.Supplement-2.47 10.1111/j.1468-0092.1990.tb00218.x doi:10.1016/j.jasrep.2019.101975 10.1371/journal.pone.0168289 doi:10.1016/j.jas.2015.06.009 10.1007/s00410-008-0323-z 10.1007/s12520-020-01050-0 10.1007/s12520-016-0447-4 10.1111/arcm.12158 doi:10.1016/S0009-2541(00)00322-3 10.1238/Physica.Topical.115a01007 10.1007/s00339-012-7341-4 doi:10.1016/j.jnoncrysol.2005.06.046 doi:10.1016/j.jasrep.2021.103082 doi:10.1016/j.sab.2006.12.002 10.1111/j.1475-4754.2011.00632.x 10.3390/heritage5010021 |
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| SubjectTerms | Archaeology Chemical composition Chemical Sciences Color Coloring colouring techniques Iron iron redox Late Antique glass Manganese or physical chemistry Oxidation Raw materials Spectrum analysis Surface layers Synchrotron radiation Theoretical and Valence X ray absorption X ray fluorescence analysis XANES XRF |
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| Title | Unravelling the role of iron and manganese oxides in colouring Late Antique glass by micro-XANES and micro-XRF spectroscopies |
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