- Open Access
Investigations by Raman microscopy, ESEM and FTIR-ATR of wall paintings from Qasr el-Ghuieta temple, Kharga Oasis, Egypt
© Mahmoud; licensee Chemistry Central Ltd. 2014
- Received: 22 August 2013
- Accepted: 6 August 2014
- Published: 29 August 2014
In the present work, a multi-analytical approach was used to analyze samples collected from the wall paintings of Qasr el-Ghuieta temple, Kharga Oasis, Egypt. The temple is dating back to the 27th dynasty (525–404 BC) and was completed during the Ptolemaic period. The samples were analyzed by optical microscopy (OM), environmental scanning electron microscopy (ESEM) coupled with an energy dispersive X-ray analysis system (EDX), Raman microscopy and Fourier transform infrared–attenuated total reflectance spectroscopy (FTIR–ATR). The chromatic palette used in the temple was identified as Egyptian blue (cuprorivaite), red ochre (haematite), yellow ochre (goethite) and carbon black (from a vegetable origin). The green pigment was identified as green earth, however, a green tonality was also obtained through a mixture of Egyptian blue and yellow ochre, and in some samples, carbon black was also found. Several amounts of anatase and carbon black were found in the red and yellow ochre samples, respectively. The analysis showed that the preparation layer is almost made of pure gypsum, while the plaster layer based mainly on gypsum with variable amounts of quartz, calcite and clay minerals. The results showed that the painting materials and techniques used in the temple are almost the same of those used in the Egyptian temples with respect to the stratigraphy of paint layers, chromatic palette and the painting technique employed.
- Qasr el-Ghuieta temple
- Kharga Oasis
- Wall paintings
- Raman microscopy
Kharga Oasis is located to the west of the Nile valley, about 550 km to the South of Cairo. Kharga, is the largest oasis of the Libyan desert and consists of a depression (about 160 km long and 20–80 km wide) (Bliss and Osing, 1985). Kharga Oasis was an important transit point for the desert caravans since the 12th dynasty (c. 1786–1665 BC) . The largest and best preserved site at Kharga Oasis is the temple of Hibis from the Persian period (c. 660–330 BC), located about two kilometres to the north of the modern city of Kharga. During the Christian period, some of the old temples and forts in the oasis were converted to churches and monasteries .
Qasr el-Ghuieta temple
The analysis of painting materials is considered an integral part of any pre-restoration research. In case of wall paintings, paint analysis usually begins with visual observation, for the purpose of locating representative areas for analysis. The optical microscopy helps in gathering information about the thickness and sequence of paint layers, colour and texture of those layers . In order to study the morphology and chemical composition of the samples, scanning electron microscopy is usually used and the elemental microanalysis by SEM–EDX is always a valuable preliminary orientation . Raman spectroscopy is a micro-analytical technique achieved several advantages in analysis of ancient painting materials. It has been successfully applied to study ancient Egyptian pigments and wall paintings -. This technique is non-destructive because little sample preparation is required or no sampling in case of micro-Raman . Raman analysis is particularly suitable for the identification of pigments in complex matrixes and inorganic pigments in artworks -. The objectives in Raman microscopy allow the laser radiation to be focused on a 1–3 μm spot typically in the visible region (in the infrared, the spot size is 10 μm and over), which is particularly useful for the identification of specific components in heterogeneous mixtures. In Fourier transform infrared–attenuated total reflectance spectroscopy (FTIR–ATR), the sample is in direct contact with the crystal that allows the infrared radiation to penetrate through the sample many times. This is due to the crystal having a high Refractive Index causing the infrared radiation to be bounced back many times. The use of ATR eliminates, in many cases, the need for sample preparation or at least simplifies the procedures.
In general, many studies have been devoted to characterize materials dating back to the Roman age from different sites around the world, some of these materials are pigments -, mortars -, and plasters . In contract of this, few studies were undertaken to study materials from Ptolemaic and Roman monuments in Egypt -. For this, the mean aim of the present work was to study pigment and plaster samples collected from the temple of Qasr el-Ghuieta, Kharga Oasis, Egypt using different analytical techniques. The obtained data will allow a comparison between wall paintings from the late period and Ptolemaic age with those from the Pharaonic age.
As a result of the deterioration factors affecting the site (mainly salt weathering), the wall decorations are suffering from exfoliation and several detachments. A total number of eleven samples (with approximate dimensions 1×1.5 to 2×2.5 cm) were carefully chosen for analysis. Also, some grains (a few milligrams) from the well preserved decorations were carefully scraped off the painted walls with a metallic scalpel. In order to get information on the startigraphy of the paint layers (mainly the blue paint layers due to the size of samples), cross-sections were prepared prior to analysis by optical microscopy and ESEM, the samples were embedded in Epoxy resin (EpoFix), cross-sectioned using variable silicon carbide papers and DP-lubricant blue for fine and cool polishing, and mounted on glass slides.
Preliminary observations on the samples were performed using an Olympus SZ-40 stereomicroscope (10 and 20× objectives) equipped with an Olympus DP10 digital camera. Optical observations on the cross-sections were carried out using an Olympus BX60 in reflection mode (with optical magnifications 50× to 500×) equipped with a JVC KY-F1030 digital camera. The optical images were captured in the reflected light which helped in identifying the structure of the paint layers and the colour of certain individual pigment grains. The prepared thin-sections of the plaster samples were examined by a Nikon Eclipse E600 microscope with photographic PixeLINK PL-A623 digital camera.
ESEM and micro X-ray analysis
The microstructure and microanalysis of the studied samples were analyzed by environmental scanning electron microscope model Philips XL-30 ESEM. This equipment is a field-emission source, offering a wide range of operating conditions, in which specimens can be examined with high chamber pressure environment. The X-ray microanalysis was carried out using an EDX detector (in a EDAX, Apollo SDD 10) with 20 Kv accelerating voltage and pressure of 3.0 Torr. EDX data acquisition was obtained through GENESIS 6.x software. Microanalysis of single pigment grains down to 1 μm, as well as of the matrix and the total average of the paint layer were performed. Also, some polished cross-sections were investigated.
Raman spectra were recorded using a Renishaw InVia Raman spectrometer in the near infrared excitation line (785 nm) of a diode laser source. The instrument is equipped with Peltier cooled charge coupled device (CCD 576x400 pixels). A Leica DMLM microscope with a XYZ motorized stage with 200 and 500 magnification objectives was equipped to the Raman spectrometer which helped in providing a sample irradiation diameter of up to 1 μm. A polarized unit system is mounted onto the microscope which offers a clear view of the area under investigation, necessary for positioning the beam on individual pigment particles. The lower laser powers (up to 0.5 mW) were used to avoid inducing thermal changes to the mineralogy of the iron oxide minerals. Typical exposure time of the CCD was 20s per scan, while normally 5 up to 20 accumulations were co-added to produce the final spectrum in order to improve the signal-to-noise ratios.
FTIR–ATR spectra were collected on a Perkin Elmer spectrometer 400 equipped with an ATR (attenuated total reflectance) detector using a diamond cell in the wavelength range of 4000–650 cm−1, at a spectral resolution of 4 cm−1 over 32 scans. A background of the clean diamond cell was performed for each analysis undertaken. The diamond cell requires only minute amounts of sample material. Also, spectra were recorded by contacting the ATR crystal directly onto the polished surfaces of the mounted cross sections.
Summary of the results obtained from different analytical techniques employed to study the samples
- Thickness =150-250 μm.
Si, Ca, Cu, S, Fe, Al, Mg
- Under reflected light: coarse heterogonous crystals (30 μm in length) with dark blue colour are observed.
- Thickness = 100-200 μm.
Si, Ca, Cu, S, Fe, Al, Mg
- It appears as pale blue probably due to the white binding medium (gypsum).
- Thickness = 150-200 μm
Si, Ca, Cu, S, Fe, Al, Mg
- Dark blue and yellow grains are observed, black grains can be seen in some areas.
- Thickness = 50-70 μm
Si, Ca, S, Fe, C, Al, K, Mg
- Several voids are spread on the surface and black grains are found.
- Thickness = 30 μm.
Si, Ca, S, Fe, Al, K, Mg
- The surface is slightly compact with red and black grains within the paint layer.
- Thickness = 30-70 μm.
C, Si, Fe, Ca, S, Cl, Na, Al, Mg, K, Ti
- Thickness = 100-200 μm.
S, Ca, Si, Al, Mg
- Thickness = 2–4 mm.
S, Ca, Si, Al
- The sample filled with angular particles.
Microstructure and microanalysis (ESEM–EDX)
Results of Raman microscopy
The blue pigment
The blue pigment was identified as Egyptian blue. The earliest recorded use of this pigment was in the IVth Dynasty (2613–2494 BC) and its use lasted throughout the dynastic period and continued on into the Roman period. For the Ptolemaic-Roman period, we have a description of the manufacture of a blue pigment, which is clearly Egyptian blue frit, given by Vitruvius (at the beginning of the 1st century BC). In addition, there is the production debris resulting from the manufacture of Egyptian blue frit at the site of Memphis, near Cairo, that dates to somewhere in the period from 3rd century BC to 3rd century AD . The optical examination on the blue paint layer showed a think pigmented layer with dark blue crystals scattered across a glassy background. For light blue areas, diluted blue is used to describe the colour of fine-textured Egyptian blue that has a large amount of glass formed in its composition, which masks the blue colour and gives it a diluted appearance. Under microscope light, and due to the white binding medium, the colour of such layers is always pale blue. The macroscopic impression however may be more intense blue. In addition, the artist probably wanted a light blue shade for this particular part of the decoration, in which case he has diluted the pigment in more white binder. From the ESEM–EDX analysis, major elements of Si, Ca and Cu were detected and FTIR–ATR analysis confirmed the presence of cuprorivaite. No Raman bands were recorded for the blue pigment samples using our spectrometer (785 nm laser). Egyptian Blue, upon excitation in the visible and NIR, exhibits strong fluorescence emission with a maximum at about 890 nm . Red and brown grains were observed in the blue paint layers, it is suggested that red ochre was added on purpose to the blue pigment to produce special hues. In his study of blue pigments from the Ptolemaic temple of Hathor at Thebes (decorated in the third century by Ptolemy IV and enhanced by Ptolemy VI and also by Ptolemy XI), Marey Mahmoud , showed that the blue pigment was identified as Egyptian blue and the micro X-ray fluorescence analysis revealed significant quantities of lead in the glass phase suggesting that a leaded bronze scrap was used to produce the pigment.
The green pigment
On the basis of ESEM–EDX and FTIR–ATR data, the green pigment was identified as green earth (Terre Verte), also, a green tonality was obtained through a mixture of Egyptian blue and yellow ochre. Such a technique of obtaining green, which appeared sporadically during the XIIth Dynasty (1991–1786 BC), became much more widespread during the Amarna period (1370–1352 BC) .
The optical observation under microscope was sufficiently enough to confirm this process since residues of the original blue and yellow pigment grains are clearly observed. Many authors have reported the detection of green earth pigments in Roman wall paintings in Egypt; in their study of the chromatic palette of the Dakke temple at Nubia dating back to the 2nd BC century Frommold et al. , reported that the green pigment was of basic copper chlorides (atacamite, CuCl2Cu(OH)2), but they claimed that they were not able to decide whether it is the originally used pigment or a secondary product of a deterioration process.
The red pigment
The red pigment was identified as red ochre (haematite). Pigments made from ochre are often discovered as long-lasting colourful remains in archaeological contexts. Raman bands recorded on the red pigment showed that a well-crystallised haematite is used. In the Raman spectrum of the pigment, anatase was detected; the most obvious possibility of the detection of this mineral is its simple presence already in the natural geological materials. Both rutile and anatase have been found by other authors in red pigment samples . Red ochre was found combined with carbon black to produce tonalities of dark red and brown.
The yellow pigment
Pigments made from ochre are often discovered as long-lasting colourful remains in archaeological contexts. In the Egyptian wall paintings, ochre pigments were widely used without interruptions from the 5th Dynasty (c. 2494–2345 BC) till the Roman period in Egypt.The yellow pigment was identified as yellow ochre (goethite) (with minor quantities of clay and quartz). Raman bands recorded on the yellow pigment showed that a well-crystallised goethite was used.
The black pigment
The black pigment was identified as carbon black. Since the characteristic band of [PO4]3− was not detected in Raman analyses and no phosphorus was found in the ESEM–EDX analysis, it is possible to exclude the animal origin of the pigment. Black pigments of vegetable origin have generally been made from various kinds of charred plant matter, mostly wood, but also leaves or seeds; the charcoal formed during the charring process is then washed, to remove soluble matter, and finally ground to powder . The analysis of black pigments from the Ptolemaic baths in front of Karnak temples complex, revealed the detection of bone black . Bone black is one of the oldest pigments known to humans, and was originally made by charring animal bones.
Preparation layer and plasters
From ESEM–EDX, micro-Raman and FTIR–ATR analyses, gypsum was identified as the main component of both the preparation and plaster layers. Many authors studied samples from wall paintings in pharaonic temples in Upper Egypt, for example: the temple of Seti I in Abydos, the 19th dynasty, c. 1293–1185 BC) , and they have reported that the decorations of these temples were applied in thin layers on a preparation layer consists of gypsum, as it was common in this period of time.
FTIR–ATR analysis on the pigment samples showed the spectra are consistent with a proteinaceous material (amide II vibration at 1541 and 1578 cm−1). The absence of carbonyl bands at c. 1730 cm−1 suggests the presence of a proteinaceous material (probably animal glue). In most of samples, the content of animal glue was not confirmed because the amide I and II bands are masked by the broad bands of calcium sulphate, oxalate and carbonate. Further analysis using gas chromatography mass spectrometry (GC/MS) will be useful to identify the proteins in the sample. From this, we suggest that tempera technique was employed in the decorations of the temple.
In this study, the complementary use of optical microscopy, Raman microscopy, FTIR–ATR and ESEM–EDX mapping on micro-samples allowed direct identification of the minerals contained in pigment and plaster samples collected from wall paintings of Qasr el-Ghuieta temple, Kharga Oasis, Egypt. The results showed that the pigments used were Egyptian blue (cuprorivaite), red ochre (haematite), yellow ochre (goethite) and carbon black (from a vegetable origin). The green pigment was identified as green earth (Terre Verte), and a green tonality was obtained through a mixture of Egyptian blue and yellow ochre, and in some samples, carbon black was also found. In particular, Raman microscopy was really helpful for identifying individual grains in both the pigment and plaster samples. Several amounts of anatase and carbon black were found in the red and yellow pigments, respectively. The analysis showed that the preparation layer was made of gypsum while the plaster samples consist of quartz, gypsum, calcite and clay minerals. No significant differences were found between the wall decorations of Qasr el-Ghuieta temple, Kharga Oasis, Egypt and those applied in the Pharaonic temples, and their chemical composition and stratigraphy are almost the same. The findings of this study are in accordance with previous analyses of ancient Egyptian pigments, which indicate the continuous use of artificial and natural earth pigments. The results will be used in the conservation–restoration interventions regarding these decorations.
The author is grateful to Mr. Alain Tonetto, Pôle PRATIM, Faculté des Sciences, Aix-Marseille Université for ESEM investigation.
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