Skip to main content Accessibility help

Mineralogical Characterization of Hispano-Moresque Glazes: A µ-Raman and Scanning Electron Microscopy with X-Ray Energy Dispersive Spectrometry (SEM-EDS) Study

  • Susana Coentro (a1) (a2) (a3), Rui C. da Silva (a4), Cátia Relvas (a5), Teresa Ferreira (a5), José Mirão (a6), Alfonso Pleguezuelo (a7), Rui Trindade (a8) and Vânia S. F. Muralha...


This work explores the combination of µ-Raman spectroscopy and scanning electron microscopy with X-ray energy dispersive spectrometry (SEM-EDS) for the study of the glazes in 15th–16th century Hispano-Moresque architectural tiles. These are high lead glazes that can be tin-opacified or transparent, and present five colors: tin-white, cobalt-blue, copper-green, iron-amber, and manganese-brown. They are generally homogenous and mineral inclusions are mostly concentrated in the glaze-ceramic interface. Through SEM-EDS, these inclusions were observed and chemically analyzed, whereas µ-Raman allowed their identification on a molecular level. K-feldspars, wollastonite and diopside were the most common compounds, as well as cassiterite agglomerates that render the glaze opaque. Malayaite was identified in green glazes, and andradite and magnesioferrite in amber glazes. Co–Ni–ferrites were identified in blue glazes, as well as Ni–Fe–olivines. Manganese-brown is the color where most compounds were identified: bustamite, jacobsite, hausmannite, braunite, and kentrolite. Through the µ-Raman analysis of different areas in large inclusions previously observed by SEM, it was possible to identify intermediate phases that illustrate the reaction process that occurs between the color-conferring compounds and the surrounding lead glaze. Furthermore, the obtained results allowed inference of the raw materials and firing temperatures used on the manufacture of these tiles.


Corresponding author

* Author for correspondence: Susana Coentro, E-mail:


Hide All

In memoriam of our co-author and dear friend V.S.F. Muralha.

Cite this article: Coentro S, da Silva RC, Relvas C, Ferreira T, Mirão J, Pleguezuelo A, Trindade R, Muralha VSF (2018) Mineralogical Characterization of Hispano-Moresque Glazes: A µ-Raman and Scanning Electron Microscopy with X-Ray Energy Dispersive Spectrometry (SEM-EDS) Study. Microsc Microanal 24(3): 300–309. doi: 10.1017/S1431927618000338



Hide All
Anthony, JW, Bideaux, RA, Bladh, KW and Nichols, MC (Eds) (2003) Handbook of Mineralogy. Chantilly, VA: Mineralogical Society of America.
Buzgar, N, Apopei, AI and Buzatu, A (2013) Characterization and source of Cucuteni black pigment (Romania): Vibrational spectrometry and XRD study. J Archaeol Sci 40(4), 21282135.
Caviró, BM (1991) Cerámica Hispanomusulmana andalusí y mudéjar. Madrid: Ediciones El Viso.
Chandramohan, P, Srinivasan, MP, Velmurugan, S and Narasimhan, SV (2011) Cation distribution and particle size effect on Raman spectrum of CoFe2O4 . J Solid State Chem 184, 8996.
Coentro, S (2017) An Iberian heritage: Hispano-Moresque architectural tiles in Portuguese and Spanish Collections. PhD Thesis, Faculdade de Ciências e Tecnologia, Universidade Nova de Lisboa.
Coentro, S, Alves, LC, Relvas, C, Ferreira, T, Mirão, J, Molera, J, Pradell, T, Trindade, RAA, da Silva, RC and Muralha, VSF (2017) The glaze technology of Hispano-Moresque ceramic tiles: A comparison between Portuguese and Spanish collections. Archaeometry 59(4), 667684.
Coentro, S, Lima, AM, Silva, AS, Pais, AN, Mimoso, JM and Muralha, VSF (2012) Pigments and pigment mixtures in Portuguese 17th century Azulejos. J Eur Ceram Soc 32(1), 3748.
Coentro, S, Trindade, RAA, Mirão, J, Candeias, A, Alves, LC, da Silva, RC and Muralha, VSF (2014) Hispano-Moresque ceramic tiles from the Monastery of Santa Clara-a-Velha (Coimbra, Portugal). J Archaeol Sci 41, 2128.
Coutinho, ML, Veiga, JP, Alves, LC, Mirão, J, Dias, L, Lima, AM, Muralha, VS and Macedo, MF (2016) Characterization of the glaze and in-glaze pigments of the nineteenth-century relief tiles from the Pena National Palace, Sintra, Portugal. Appl Phys A 122, 696.
Freeman, JJ, Wang, A, Kuebler, KE, Jolliff, BL and Haskin, LA (2008) Characterization of natural feldspars by Raman spectroscopy for future planetary exploration. Can Mineral 46(6), 14771500.
Gratuze, B, Soulier, I, Blet, M and Vallauri, L (1996) De l’origine du cobalt: du verre à la céramique. Revue d’Archéométrie 20, 7794.
Kamble, RB, Varade, V, Ramesh, KP and Prasad, V (2015) Domain size correlated magnetic properties and electrical impedance of size dependent nickel ferrite nanoparticles. AIP Adv 5(1), 17119.
Kim, J, Choi, KJ, Bahn, CB and Kim, JH (2014) In situ Raman spectroscopic analysis of surface oxide films on Ni-base alloy/low alloy steel dissimilar metal weld interfaces in high-temperature water. J Nucl Mater 449, 181187.
Lin, CC (2001) Vibrational spectroscopic study of the system α-Co2SiO4 - α-Ni2SiO4 . J Solid State Chem 157(1), 102109.
Machado, A and Vilarigues, M (2016) Cobalt blue – Reproduction and characterisation of blue enamel recipes from The Handmaid to the Arts by Robert Dossie. Glass Technol Eur J Glass Sci Technol A 57(4), 131140.
Majumdar, MG (2012) Analysis of stress-coupled magneto-electric effect in BaTiO3-CoFe2O4 composites using Raman spectroscopy. Int J Sci Eng Res 3(11), 17.
Molera, J, Pradell, T, Martinez-Manent, S and Vendrell-Saz, M (1993) The growth of sanidine crystals in the lead of glazes of Hispano-Moresque pottery. Appl Clay Sci 7(6), 483491.
Molera, J, Pradell, T, Salvadó, N and Vendrell-Saz, M (2001) Interactions between clay bodies and lead glazes. J Am Ceram Soc 84(5), 11201128.
Molera, J, Pradell, T, Salvadó, N and Vendrell-Saz, M (2009) Lead frits in Islamic and Hispano-Moresque glazed productions. In From Mine to Microscope: Advances in the study of Ancient Technology, Shortland, AJ, Freestone, I and Rehren, T (Eds.) pp. 110. Oxford: Oxbow Books.
Molera, J, Coll, J, Labrador, A and Pradell, T (2013) Manganese brown decorations in 10th to 18th century Spanish tin glazed ceramics. Appl Clay Sci 82, 8690.
Molera, J, Vendrell-Saz, M, García-Vallés, M and Pradell, T (1997) Technology and color development of Hispano-Moresque lead-glazed pottery. Archaeometry 39(1), 2339.
Mouri, T and Enami, M (2008) Raman spectroscopic study of olivine-group minerals. J Mineral Petrol Sci 103, 100104.
Mulholland, IR (1984) Malayaite and tin-bearing garnet from a skarn at Gumble, NSW, Australia. Mineralogical Mag 48(48), 2730.
Navarro, JMF (2003) El Vidrio. Madrid: Consejo Superior de Investigaciones Científicas/Sociedad Española de Cerámica y Vidrio.
Piña, C, Arriola, H and Nava, N (2005) Study of malayaite and malayaite cobalt pigment. Hyperfine Interact 161(1–4), 9397.
Pleguezuelo Hernández, A (2003) Lozas y Azulejos de la Colección Carranza (2 vol) Castilla-La Mancha: Junta de Comunidades.
Pradell, T, Molera, J, Salvadó, N and Labrador, A (2010) Synchrotron radiation micro-XRD in the study of glaze technology. Appl Phys A 99, 407417.
Ricciardi, P (2008) Raman spectroscopy for the non destructive characterization of ancient pottery, porcelains and mosaic glasses, Università degli Studi di Firenze.
RRUFF (2016) RRUFF™ project. Available at (retrieved October 10, 2016).
Trindade, RAA (2007) Revestimentos Cerâmicos Portugueses. Meados do século XIV à primeira metade do século XVI. Lisboa: Edições Colibri/Faculdade de Ciências Sociais e Humanas da Universidade Nova de Lisboa.
Vieira Ferreira, LF, Conceição, DS, Ferreira, DP, Santos, LF, Casimiro, TM and Ferreira Machado, I (2014) Portuguese 16th century tiles from Santo António da Charneca’s kiln: A spectroscopic characterization of pigments, glazes and pastes. J Raman Spectrosc 45, 838847.
Zhang, Z and Saxena, SK (1991) Thermodynamic properties of andradite and application to skarn with coexisting andradite and hedenbergite. Contrib Mineral Petrol 107(2), 255263.
Zucchiatti, A, Bouquillon, A, Katona, I and D’Alessandro, A (2006) The ‘Della Robbia blue’: A case study for the use of cobalt pigments in ceramics during the Italian Renaissance. Archaeometry 48(1), 131152.
Zuluaga, MC, Alonso-Olazabal, A, Olivares, M, Ortega, L, Murelaga, X, Bienes, JJ, Sarmiento, A and Etxebarria, N (2012) Classification of glazed potteries from Christian and Muslim territories (Late Medieval Ages, IX–XIII centuries) by micro-Raman spectroscopy. J Raman Spectrosc 43, 18111816.


Mineralogical Characterization of Hispano-Moresque Glazes: A µ-Raman and Scanning Electron Microscopy with X-Ray Energy Dispersive Spectrometry (SEM-EDS) Study

  • Susana Coentro (a1) (a2) (a3), Rui C. da Silva (a4), Cátia Relvas (a5), Teresa Ferreira (a5), José Mirão (a6), Alfonso Pleguezuelo (a7), Rui Trindade (a8) and Vânia S. F. Muralha...


Altmetric attention score

Full text views

Total number of HTML views: 0
Total number of PDF views: 0 *
Loading metrics...

Abstract views

Total abstract views: 0 *
Loading metrics...

* Views captured on Cambridge Core between <date>. This data will be updated every 24 hours.

Usage data cannot currently be displayed