Painting the Palace of Apries II: Ancient Pigments of the Reliefs From

Hedegaard et al. Herit Sci (2019) 7:54 https://doi.org/10.1186/s40494-019-0296-4 RESEARCH ARTICLE Open Access Painting the Palace of Apries II: ancient pigments of the reliefs from the Palace of Apries, Lower Egypt Signe Buccarella Hedegaard1, Thomas Delbey2, Cecilie Brøns1 and Kaare Lund Rasmussen2* Abstract Fragments of painted limestone reliefs from the Palace of Apries in Upper Egypt excavated by Flinders Petrie in 1908–1910 have been investigated using visible-induced luminescence imaging, micro X-ray fuorescence, laser ablation inductively coupled plasma mass spectrometry, micro X-ray powder difraction, and Fourier transform infrared spectrometry. The pigments have been mapped, and the use and previous reports of use of pigments are discussed. Mainly lead–antimonate yellow, lead–tin yellow, orpiment, atacamite, gypsum/anhydrite, and Egyptian blue have been detected. It is the frst time that lead–antimonate yellow and lead–tin yellow have been identifed in ancient Egyptian painting. In fact, this is the earliest examples known of both of these yellow pigments in the world. Keywords: Ancient Egyptian polychromy, Apries Palace, µ-XRF, LA-ICP-MS, µ-XRPD, FTIR, VIL, Lead–antimonate yellow, Lead–tin yellow, Orpiment, Atacamite, Egyptian blue Introduction the published investigations of wall paintings throughout Tis paper constitutes the second and fnal article in ancient Egyptian history, almost exclusively cover exam- the series on the technical examination of the painted ples from temples, tomb-chapels, and burial chambers. fragments from the so-called Palace of Apries housed Tus, the investigation of the Palace of Apries consti- in the collection of the Ny Carlsberg Glyptotek (NCG). tutes a signifcant contribution to our understanding of Whereas the frst article focuses on the organic compo- painted decoration from the Late Period as well as to our nents [1], this article deals with the pigments used. knowledge of wall paintings in relation to secular prestige Although the number of technical studies of ancient buildings. Egyptian painting is increasing, it is still infnitesimal Although pigments are generally inorganic, a few dye- considering that it pertains to a period spanning thou- based pigments were in use in antiquity. Tese include sands of years. Te majority of the published studies semi-organic pigments, such as lakes based on mad- focus on material from the New Kingdom [2–5] and the der (multiple dyestufs incl. C14H8O4 and C15H8O7), and 1 Greco-Roman Period [6]. Tus, our knowledge is quite organic pigments, such as indigo (C 16H10N2O2). Many limited concerning painting and pigments from the inter- organic pigments can be detected by gas chromatogra- vening seven centuries generally referred to as the Tird phy mass spectrometry (GC–MS)—a technique which Intermediate Period (c. 1070–664 BCE) and the Late has been applied to the samples in the frst paper of this Period (c. 664–332 BCE). Furthermore, most of the stud- sequel [1]. Te GC–MS data did not reveal the pres- ies published from these less elucidated periods focus on ence of any organic pigments. In the present work, the cofns and papyri rather than wall paintings. Moreover, 1 Te APPEAR (Ancient Panel Paintings: Examination, Analysis, and *Correspondence: [email protected] Research) Project investigates mummy portraits from Roman-era Egypt. 2 CHART, Institute of Physics, Chemistry and Pharmacy, University Technical information is gathered from multiple collections worldwide and of Southern Denmark, Odense, Denmark made available through an online database. See: http://www.getty .edu/museu Full list of author information is available at the end of the article m/resea rch/appea r_proje ct/. © The Author(s) 2019. This article is distributed under the terms of the Creative Commons Attribution 4.0 International License (http://creat iveco mmons .org/licen ses/by/4.0/), which permits unrestricted use, distribution, and reproduction in any medium, provided you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons license, and indicate if changes were made. The Creative Commons Public Domain Dedication waiver (http://creat iveco mmons .org/ publi cdoma in/zero/1.0/) applies to the data made available in this article, unless otherwise stated. Hedegaard et al. Herit Sci (2019) 7:54 Page 2 of 32 chemical composition of the inorganic pigments is inves- natural calcium sulphates are widely available in Egypt tigated. In order to keep sampling to a minimum, the [3, 4, 6]. When heated to c. 90 °C, gypsum converts to investigation is largely based on non-invasive measures hemihydrate (2CaSO4·2H2O), whereas it is converted incl. microscopy, photographic techniques, and micro- to anhydrite when heated to 200 °C. Te fact that these X-ray fuorescence spectroscopy (µ-XRF). Laser ablation dehydrated phases are sometimes found in ancient inductively coupled plasma mass spectrometry (LA-ICP- Egyptian ground layers indicates that the gypsum has MS), micro-X-ray powder difraction (µ-XRPD), and Fou- been heated. However, since mixtures of anhydrite and rier transform infrared spectrometry (FTIR) have been gypsum occur in natural deposits [6, 7], the dehydrated carried out, on single samples, in order to resolve compo- phases may have formed as a result of anthropogenic sitional complexities. intervention or geological processes. Considering that the fragments have lain buried in Furthermore, the magnesium calcium carbonate min- the ground for millennia, the inorganic pigments identi- eral huntite (Mg 3Ca(CO3)4) has also been attested in fed in this study have undergone very little degradation. several cases dating from the Old Kingdom onwards. It could, however, be speculated that organic colorants Huntite is an outstanding painting material which pro- might have been present, but have now been lost due to vides a brighter white than calcite and ensures a smooth degradation. Although this is theoretically possible from painted surface due to its adhesiveness and small particle a chemical point of view, there are no indications in the size. Although used less extensively than the other white art historical context or from visual appearance of the pigments, recent studies suggest that the use of huntite architectural fragments that a colourant is missing. In was more wide-spread than previously thought. In fact, fact, the polychromy is so well-preserved that GC–MS it appears to have been the predominant white pigment analyses have yielded detailed information on the organic during the New Kingdom (18th, 19th and 20th Dynas- components used as binders and coatings [1]. ties) [3, 7]. Huntite is structurally and chemically similar to calcite, magnesite (MgCO 3) and dolomite ([Ca,Mg] Ancient Egyptian pigments: a review [CO3]2). It occurs as soft, white, fne-grained, compact Comparative studies are made difcult by the lack of and porous masses which crumble easily. Huntite typi- relevant pigment studies from the Tird Intermedi- cally forms as an alteration product of dolomite- and ate Period and the Late Period. Te few published stud- magnesite-bearing rocks. It can also form via precipita- ies focusing on pigments from the said periods typically tion in vugs, caves, and fault zones [8]. treat of artefacts such as papyri and cofns which difer signifcantly in size, function, and materials—and there- Blue pigments fore in painting techniques and pigment palettes. For this Te principal blue pigment employed in ancient Egypt reason a review of the pigments thus far attested on arte- is the synthetic pigment today known as Egyptian blue. facts contemporary to the Palace of Apries would not be Whether invented in Mesopotamia or Egypt, the pigment meaningful in this context. Albeit our current knowledge was evidently in use in Egypt from the early 3rd millen- of ancient Egyptian wall painting is based on architec- nium BCE [8, 9]. Manufacture seems to have quickly tural structures predating the fragments examined in this gained momentum from that time and archaeological study, this knowledge is deemed more relevant for the evidence supports the hypothesis that the production of assessment of the palette used for wall decorations in the Egyptian blue continued in Egypt until at least the third Tird Intermediate Period and the Late Period. Tus, due century CE [3, 10]. Te pigment is prepared from a mix- to lack of information on contemporary wall painting, ture of quartz, lime, a copper compound, and an alkali the pigments so far identifed in ancient Egyptian paint- fux which is fred at temperatures around 850 to 1000 °C. ing, up to and including the Late Period, are included in Te principal components of Egyptian blue are blue cal- the present review. cium-copper tetrasilicate crystals [synthesised cuprori- vaite (CaCuSi4O10)] and partially reacted quartz particles White pigments bonded together by a glass phase [9]. Calcite (CaCO3), gypsum (CaSO4·2H2O) and anhydrite Widely recorded in painted archaeological materials, (CaSO4) are the most common pigments in painted Egyptian blue was clearly in routine use as a standard decoration in ancient Egypt from the Predynastic Period blue pigment of Egyptian art [4, 8]. In fact, other blue pig- through the Roman Period. First and foremost, these ments account for a miniscule proportion of the count- white pigments were used for the ground layer often less examples of blue in ancient Egyptian polychromy. serving as the preparatory layer as well as the back- Tus, azurite (Cu3(CO3)2(OH)2), a natural bright blue ground colour. In addition, they were used for the paint carbonate of copper which was widely used from Antiq- layers applied on top of the ground layer. Calcite and uity until the end of the seventeenth century [8], occurs Hedegaard et al. Herit Sci (2019) 7:54 Page 3 of 32 extremely rarely in Egyptian contexts [4]. In fact, the Furthermore, green copper chlorides such as atacamite only confrmed example is a fragment of painted leather (Cu2Cl(OH)3) and other mineral species in the atacamite from the Asaif Valley at Tebes.

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