KIRSTEN TRAVERS

ARTC 673 ADVANCED ANALYTICAL TECHNIQUES

A TECHNICAL ANALYSIS OF THE TURKISH ROOM CEILING
MAY 21, 2010

MATERIALS: wood, paint, metal leaf, mirrors

DATE: late 18th century
DIMENSIONS: 144 x 159
ORIGIN: Damascus, Syria
CURRENT LOCATION: Shangri La estate; Honolulu, HI

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

ABSTRACT: The Turkish Room ceiling once functioned as part of an elaborate 18th century interior in Damascus, and was

decorated with paint, metal leaf, and raised gesso ornaments known in Arabic as `adjami. To elucidate the ceilings original
appearance and Damascene craft techniques, decorative materials were analyzed using cross-section microscopy and polarized
light microscopy (PLM), as well as instrumental techniques including energy-dispersive x-ray fluorescence spectroscopy (EDXRF), energy dispersive x-ray microanalysis in the scanning electron microscope (SEM-EDS), scanning electron microscopy
with backscattered electron imaging (SEM-BSE), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, and
gas chromatography mass spectrometry (GC-MS). The results show the `adjami is composed of gypsum in animal glue, while
tinted natural resins were used to give tin leaf a golden appearance. A variety of pigments and binding media were also
characterized, including copper resinates, smalt in an egg binder, and a pink paint made with white lead in oil which may retain
the fragments of cochineal or kermes insects used to prepare the red colorant. Restoration materials identified with this analysis
include a later natural resin varnish, a green synthetic paint, and an industrial-strength pesticide.

1. INTRODUCTION
The Turkish Room at Shangri La is a pastiche of architectural elements including wall panels, doors, and marble
inlaid floors, all of which originate from Syria. Archival records show that most of these pieces, including the
ceiling, were commissioned in the 18th-century by the aristocratic Quwwatli family for the decoration of their home
in the ancient city of Damascus. The ceiling would have functioned as part of an elaborate polychrome reception
room used to receive guests in an atmosphere of wealth and luxury (figs. 1a & 1b). Consistent with Islamic style of
the period, the walls and ceilings were decorated with elaborate floral and geometric patterns using brightly colored
paints, metal leaf, and raised gesso ornaments known in Arabic as `adjami. The overall effect created a glittering,
jewel-like atmosphere which set the stage for social entertainments enhanced by music, hookah-pipe smoking, and
culinary delicacies. A similar Damascene interior was described by an Englishman in 1812, who wrote: On
entering, the eye was struck by the glitter of the walls and ceiling, resembling the description of fairy palaces. Mock
precious stones, mirrors, gilding, and arabesque paintings covered it everywhere (Keenan 2000, 96).

In 1920, The Quwwatli family sold the ceiling and related architectural elements to the Syrian art dealers Asfar &
Sarkis, who then re-sold the interior to Hagop Kevorkian, a New York-based art dealer and archaeological scholar,
in 1936. For almost four decades the ceiling and other associated elements remained in storage as Kevorkian
attempted unsuccessfully to sell the room. After Kevorkian passed away in 1969, the pieces were donated to the
newly constructed Kevorkian Center for Middle Eastern Studies at New York University (NYU). In 1976, the
iconic American heiress Doris Duke purchased the Quwwatli house elements from NYU to use in a new period
room at her Islamic-themed Shangri La estate in Honolulu, HI (fig. 1c).

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

Fig. 1a. Circa 1830 reception room

in Bait Nizam, Damascus

Fig. 1b. Circa 1840 reception room

in Bait Mujallid, Damascus

Fig. 1c. View of Shangri Las Turkish

Room from the foyer

The `adjami phenomenon was unique to Damascus, and it has been estimated that between the 17th and 19th
centuries, thousands of `adjami rooms existed within the walls of the ancient city. Sadly, many of these have been
lost to renovation, demolition, and neglect. Today, fewer than 70 survive in a precarious state of preservation.
Passed on through oral tradition, the techniques used to craft these spaces have vanished as well. As a result,
contemporary Damascene craftsmen who create rooms in this style utilize modern materials such as acrylic and
bronze paints, with little knowledge of how the rooms were decorated historically (Scharrahs, date unknown).

1.2 MATERIALS AND CONSTRUCTION: The current body of information regarding materials and construction
used to create the Turkish Room ceiling is gleaned from in-situ visual examination carried out by the author
(summer 2009), and written descriptions of other `adjami interiors in Western museums including the Damascus
Room at Shangri La (19th c.), the Aleppo Room in Berlin (c.1600), the Damascus Room in the Dresden Staatliches
Museum (c.1810), and the Nur al-Din Room at the Metropolitan Museum of Art (c.1707).

The wood beams, panels, squinches (corner pendants), and cornices comprising the ceiling would have been
constructed and decorated separately, then assembled on-site to create the whole piece (Paccard, 1980). At this
time, it is not known what woods were used to construct the Turkish Room ceiling, but other `adjami rooms were

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

made from poplar and/or walnut (Daskalakis-Mathews, 2000). The method of joinery in the Turkish Room is
unclear because the ceiling could not be examined from the reverse, but examination from the recto indicates that
glue and nails played a heavy part in its construction. During the examination, it was observed that large cracks in
the beams and in-between adjacent wood planks were filled with loamy materials or thick plant fibers soaked in glue
to create a flush surface for painting. Next, a white ground consisting of gypsum in animal glue was applied to the
surface of the wood to prepare for subsequent decorative layers (Scharrahs 2009). To create the `adjami ornaments,
a thicker mixture of gypsum, water, and animal glue was prepared (Scharrahs 2009). This viscous mixture was
dripped from a stick to create the astonishingly consistent geometric, and floral patterns seen throughout the ceiling.

In-situ examination showed that a white metal foil was applied over large areas of the ceiling. This foil exhibited a
dull, grayish-white surface corrosion and was visually similar to the metal foil in the adjacent Damascus Room,
which had been identified as tin with XRF (Leoblich and Bagnall, 2005). This extensive use of tin foil, only portions
of which are exposed in the final decorative scheme, would have allowed the craftsman to avoid the time
consuming process of gilding individual details at the end of the project. In addition, tin foil - being less expensive
than gold or silver leaf - was a more economical choice for decorating such a large surface area. The size used to
adhere the tin foil is unknown, but oil-based mordants were commonly used to adhere tin foil in other `adjami
rooms (Scharrahs, date unknown). Consequently, the use of an oil mordant would indicate that the foil was not
burnished after it was laid down (Nadolny 2006). Wrinkles and folds in the Turkish Room ceiling indicate that
burnishing was not carried out, suggesting that an oil mordant was used.

In-situ examination suggests that yellow and red translucent glazes were applied to the tin foil to impart a gold or
copper lustre to the surface. This coating is ambiguously described as lacquer or glaze in various sources, none
of which have successfully identified its material composition (Loeblich and Bagnall 2005, 7; Scharrahs 2009, 6).
The use of colored glazes over tin was described by Cennini in the 15th century, who refers to this glaze as vermeil
(Cennini 15th c., 61). Cenninis vermeil recipe refers to an oil glaze colored yellow with saffron. On various

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

polychrome objects, tin foil has reportedly been glazed with shellac, gum, or resins colored with various yellow dyes
or red lakes to mimic more precious metals (Evans 2008).

Visual examinatation determined that six paint colors were used to decorate the Turkish Room ceiling: white, black,
blue, red, pink, and green. These colors were rarely mixed. The pigments used in other `ajami interiors have been
reported as lead white, smalt, minium, vermillion, indigo, and orpiment (Scharrahs 2009). Greens were usually
copper-based but could have been created by mixing indigo with orpiment, and pinks were produced by mixing lead
white with a red madder lake (Scharrahs 2009). It is unknown what analytical techniques the author used to identify
pigments.

Combinations of binding media were used in the same room to juxtapose glossy and matte surface textures. For
instance, in the Dresden Damascus Room, cross-section microscopy, fluorochrome staining, and FTIR
demonstrated that while most paints were composed of an oil and animal glue emulsion, the orpiment and smalt
pigments were bound with animal glue only (Scharrahs, date unknown). In the same study, Scharrahs also notes that
a mixture of proteins, oils, and resins were used at the Aleppo Room in Berlin. At Shangri Las Damascus Room,
paint samples were examined with cross-section microscopy, and analyzed with fluorochrome stains. Results
suggested an emulsion of proteins and oils to create a binding medium for some paints (Loeblich and Bagnall 2005,
32-34). It is important to consider that the deliberate use of various binding media to create surface effects suggests
that `ajami rooms were not originally varnished, as this coating would have destroyed the effects so carefully created
by the craftsmen (Scharrahs, personal comment). Therefore, varnishes found over `ajami surfaces are considered
unoriginal.

1.3 PREVIOUS RESTORATION: The Turkish Room ceiling appears to have undergone numerous restoration
campaigns including localized filling and repainting to compensate losses in the `ajami ornament, as well varnishing
to saturate faded colors. While some of these restorations may have occurred when the ceiling was installed in

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

Damascus, others could have been carried out in the early 20th century by art dealers to make the rooms presentable
for sale.
Written resources and oral histories (Littlefield 1999, Travers and Barnes 2009), relate that the ceiling was restored
by Doris Duke and her staff when it arrived in Honolulu, although the precise materials used were not specified.
Visual examination suggests that loose wooden elements were repaired with an epoxy resin or hot glue, while
lacunae were hastily inpainted with a glossy paint which rarely matches the surrounding areas.

1.4 CONDITION AND TREATMENT: The decorative surfaces of the Turkish Room ceiling were found to be in a
severely deteriorated state during the 2009 examination. Most noticeably, the colors are altered significantly from
their original appearance. For instance, white paints have yellowed, pink paints have faded almost completely, green
paints have a brown tone, and blues have shifted to black. In addition, patterns of cracking, flaking, and loss were
observed in the `ajami, paints, and glazes. Varnishes have darkened with age, further distorting the original colors
and obscuring surface detail. In many areas, this varnish has reticulated, pulling up delicate glaze and metal leaf
layers and exposing the ground beneath. Consolidation treatment was carried out by WUDPAC interns LeeAnn
Barnes and the author during the summer of 2009. Flaking `ajami was consolidated with BEVA gel, a water-based
dispersion of ethylene-vinyl acetate bulked with methyl cellulose. Thin, friable flakes of paint were consolidated with
Aquazol 500 (poly 2-ethyl-2-oxazoline). Neither of these consolidants contaminated this study.

1.5 LITERATURE REVIEW: Few English-language sources discuss the analysis of `ajami interiors, making it
necessary to supplement literature research with articles related to paints or painted architectural surfaces from the
Middle East, with a particular focus on Islamic art materials or techniques contemporary with the Turkish Room
ceiling.

Purinton and Watters analyzed the pigments used in 15th to 17th-century Persian miniature paintings at the Los
Angeles County Museum of Art and compared their results with treatises on Persian painting and paint-making
techniques (Purinton and Watters 1991). Their technical analyses included x-ray fluorescence (XRF), infrared

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

reflectography (IR), x-ray diffraction (XRD) and polarized light microscopy (PLM), although they fail to specify
which technique was used for each pigment. Their results showed that the Persian palette consisted of inorganic
pigments from both mineral ores and synthetic manufacture, clays, organic pigments derived from vegetable and
insect sources, and lake pigments. The most common pigments identified were ultramarine blue and white lead.
Additional blues included azurite and indigo. Red lakes including kermes, madder, and cochineal were identified,
while inorganic red sources included hematite, red lead, and cinnabar and/or vermillion. The most common yellow
pigment found was orpiment, followed by yellow ochre. Copper based greens were identified as brochantite and
verdigris, although some greens were created with a combination of orpiment and an organic blue. All white colors
were lead based. Contrary to the literature, all blacks were found to contain charcoal rather than lampblack.

Burgio et al. applied Raman microscopy and X-Ray Fluorescence (XRF) techniques to the analysis of pigments
extent in Islamic manuscripts dating from the 16th - 18th centuries at the Victoria and Albert Museum (Burgio et al.
2008). Each manuscript was found to contain lazurite ((Na,Ca)8[(Al,Si)12O24]Sn, strong bands at 548 and 1096 cm-1),
orpiment (As2S3, bands at 353, 309, 292, and 154 cm-1), red lead (Pb3O4, bands at 548, 390, 223, 149 and 122 cm-1),
vermillion (HgS, bands at 343 and 285 cm-1, strong band at 253 cm-1), and a carbon black (broad bands at ~1580
and 1325 cm-1). Other pigments found include realgar, lead white, and copper based greens such as malachite and
atacamite. Some pigments could not be characterized and were assumed to be organic dyes. Building on the
research previously carried out by Purinton and Waters, Burgio et al. found that the Persian palette remained
relatively constant as pigment technologies evolved over the centuries. A similar approach will be used to study the
ceiling pigments, and the data reported in this article will be used for comparison as Raman and XRF results are
interpreted.

Lazzarini and Schwartzbaum carried out a technical examination of the original and restoration materials used on
the decorated dome of the 14th-century Al Asqua Mosque in Jerusalem (Lazzarini and Schwartzbaum 1985). X-ray
diffraction (XRD) was used to identify the inorganic components of the ground and pigments. The ground layer
was identified with XRD as gypsum (CaSO4 2H2O), or anhydrite (CaSO4). Paint pigments identified with XRD

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

included white lead, vermilion, red and burnt ochre, azurite, indigo, orpiment, malachite, verdigris, and a carbon
black. Red and violet lakes were also observed, but as non-crystalline materials, they could not be classified with
XRD. The restoration materials were analyzed and found to include white lead, minium, bitumen, Prussian blue,
and chrome green. Although XRD analysis is not proposed for the Turkish Room ceiling study, a combination of
XRF, SEM-EDS, FTIR, and Raman spectroscopy should identify extant pigments with the same degree of
confidence.

Phase II of the Damascus Room conservation project at Shangri La was carried out by WUDPAC fellows Amelia
Bagnall and Natasha Loeblich, under the direction of Associate Professor Richard Wolbers, and the scientists at the
Winterthur Museums Scientific Research and Analysis Laboratory (SRAL). The decorative surfaces were
characterized with cross-section microscopy, fluorochrome staining, Fourier transform infrared spectroscopy
(FTIR) and scanning electron microscopy energy dispersive spectroscopy (SEM-EDS) to identify the varnishes,
pigments, and binding media present in the room. FTIR revealed that the ground is gypsum based (peak at 1100
cm-1) with a proteinaceous binder (1450, 1550 cm-1). Discolored varnishes displayed peaks consistent with an
emulsion varnish composed of a natural resin (3300, 2900, 2800, 1700 cm-1) and protein (1550, 1450 cm-1). SEMEDS identified the white metal leaf as tin with a minor silver component, while small peaks for sulfur suggest
tarnish in the metal. The pigments were not analyzed extensively, although white lead, ultramarine (Si), and lake
pigments (Al, K) were tentatively identified with SEM-EDS (Loeblich and Bagnall 2005). These results will prove
useful to the upcoming technical study, not only as a comparative interior but because their analysis was also carried
out at Winterthurs SRAL, using the same instruments proposed for the current analysis.

The Metropolitan Museum of Art successfully identified paint and `adjami media in the Nur al-Din Room using an
immunological technique known as enzyme-linked immunosorbent assay (ELISA), (Arslanoglu and Schultz 2009).
This process uses antibodies tagged with enzymes to differentiate proteins and gums with more specificity than IR
techniques. Their analysis found that ovalbumin, a protein present in egg, was exclusively used to bind smalt
pigments, while the `adjami was bound with collagen. Although the ELISA technique is not proposed for the ceiling

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

analysis, organic materials can be classified with fluorochrome stains, FTIR, or ATR. If more specific identification
is required, quantitative GC-MS could be carried out with comparable results.
1.6 OBJECTIVE: Few analytical studies have focused on the materials used to create historic `adjami interiors.
Therefore, the Turkish Room presents a rare opportunity to contribute to the subject through analysis of an
authentic Damascene ceiling decorated in the `ajami style, using cross-section microscopy and fluorochrome
staining, complemented by the most up-to-date scientific techniques available at the Winterthur Museums Scientific
Research and Analysis Laboratory (SRAL), including energy-dispersive x-ray fluorescence spectroscopy (ED-XRF),
scanning electron microscopy with energy dispersive x-ray spectroscopy (SEM-EDS), Fourier transform infrared
spectroscopy (FTIR), Raman spectroscopy, and gas chromatography-mass spectrometry (GC-MS). The combined
results will be used to identify the ceilings original materials including paints, `ajami ornaments, metal leaf, and
glazes, permitting comparison to other `ajami interiors discussed in the literature, while elucidating 18th century
`ajami techniques. This information will also be used to reconstruct part of the ceilings original appearance and
offer explanations for the observed color shift and deterioration of decorative surfaces. Restoration materials will
also be analyzed to assign a general time period to their application, allowing the history of the ceiling to be better
understood. Finally, the findings will provide Shangri La with important data regarding one of the largest and most
important objects in their collection, and may lend themselves to making more appropriate recommendations for its
interpretation, exhibition, and treatment in the future.
1.7 EXPERIMENTAL DESIGN
First, energy dispersive x-ray fluorescence spectroscopy (ED-XRF) was used to analyze the elemental composition
of uncast fragments of metal leaf used on the Turkish Room ceiling. XRF is a non-destructive technique used for
qualitative and quantitative analysis of inorganic pigments and metals, although it is unable to provide data for
organic materials such as wood, protein, natural resins, or dyes. Loeblich and Matsen used a portable XRF
instrument to determine the alloy composition of metal leaf used at The Breakers, a mansion in Newport, Rhode
Island (Loeblich and Matsen 2006). However, XRF can penetrate hundreds of microns below the surface of a
material, so resulting spectra can be ambiguous in respect to depth.

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

Next, cross-section microscopy used to examine paint stratigraphies, specifically the quantity, color, and
morphology of decorative layers. This will be followed by examination in ultraviolet light (UV) to further
characterize layers based on their autofluoresecent behaviors. Fluorochrome staining may suggest the presence of
lipids, carbohydrates, or proteinaceous binding materials within a particular layer (Wolbers and Landrey 1987).
These techniques provided preliminary information to guide future instrumental analyses. Where applicable,
mounted cross-sections were re-used for SEM-EDS, ATR, and Raman spectroscopy.

Elemental analysis of mounted cross-sections was carried out under a range of magnifications (200-2000x), with
SEM-EDS and SEM-BSE. This technique was used to generate stratigraphic elemental maps for the
characterization of pigments, lake bases, metal foils, or metal driers. In the SEM, qualitative spot analysis can be
carried out to obtain spectra for an individual pigment particle within the paint matrix, and quantitative data can be
obtained when these results are compared to standards of known composition. This technique was used to study
smalt pigments in oil paint media in an attempt to explain degradation mechanisms (Spring et al. 2005). In addition,
SEM-BSE images map the cross-section in grayscale according to relative atomic number (Z). Higher Z elements
will appear white, while lower Z elements and organic materials will appear dark. This technique helps locate leadbased pigments (Z=82) as well as thin oil or resin layers that may be less visible with traditional cross-section
microscopy. Pigment characterizations with SEM-EDS will be supplemented by FTIR, Raman spectroscopy, and
PLM.

Fourier-transform infrared spectroscopy (FTIR- transmission mode), uses an infrared source to study the vibrations
of molecular functional groups as energy is absorbed by a sample. This technique will expand on pigment and
ground layer identifications made via SEM, but it was primarily used to classify organic materials into five
categories: oils, natural resins, waxes, proteins, and polysaccharides. This data helped characterize binding media and
various pigments, the mordant used to adhere the metal leaf, the composition of ground and `adjami, as well as
varnishes that were applied to the ceiling. Unknowns were identified through comparison to spectra of known

10

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

compounds, available in print or online sources. FTIR has proven useful for the identification of modern pigments
and synthetic resins (Lerner 2004), which assisted in the examination of recent restorations.
Attenuated total reflectance spectroscopy (ATR) was attempted to obtain spectra from layers in a mounted crosssection that cannot be separated from the bulk sample for FTIR transmission mode analysis. This technique was
used successfully to map the distribution of organic binding media and inorganic pigments within paint crosssections from 15th century Italian and German paintings in the National Gallery (Spring et al. 2008). For the Turkish
Room ceiling, this technique was proposed to characterize the colored glazes over the tin foil and paint media,
which would be difficult to separate from the larger cross-section. It should be noted that pigments containing
oxides and sulfides (such as vermillion, HgS), cannot be detected with FTIR/IR, and should be analyzed with
Raman spectroscopy, which is often used to complement FTIR data.

Raman spectroscopy uses visible and near-IR lasers to study the scattering phenomena of polarizeable organic and
inorganic materials. The intensity of Raman scattering is directly proportional to vibrational transitions in a molecule
(in this way it is complementary to FTIR), but response is also dependent on incident laser wavelength or analyte
concentration. This technique was used to support pigment identifications revealed with SEM-EDS and IR
methods, providing distinct spectral peaks which can be compared to spectra of known composition. This
technique was used to analyze the composition of inorganic pigments and lake bases. This technique was used by
Sister Daniila et al. (2000) to identify carbon black, calcium carbonate, azurite, and ochres in Byzantine frescos to
characterize original materials and distinguish them from restorations. A major advantage of Raman is that this
method can be carried out on paint cross-sections as well as those flattened on a diamond cell for FTIR, which
minimized sample preparation time during the study.

Gas chromatography mass spectrometry was the final instrumental technique used. Following derivitization and
volatilization, GC-MS can separate organic mixtures into distinct, identifiable fragments which are then analyzed
with a mass spectrometer. This technique is destructive but can yield much more specific information than
classifications obtained by FTIR alone. For instance, this technique can differentiate between egg or animal proteins

11

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

through amino acid analysis, or differentiate drying oils based on ratios of fatty acid ethyl esters (Stuart 2007). GCMS was used to analyze the binding media, glazes, varnishes, and other materials used on the ceiling where previous
analyses were ambiguous.

Polarized light microscopy was used to examine dispersed pigment samples mounted on a glass slide with Cargille
meltmount (refractive index = 1.66) to provide confirmatory evidence if instrumental analysis was inconclusive.
Characterizations were made according to optical properties such as color in transmitted light, morphology, surface
topography, birefringence, Becke line, and refractive index. Observations were compared to reference standards as
well as literature sources (Gettens and Stout 1942, Eastaugh et al. 2008).

2. EXPERIMENTAL PROCEDURES
2.1 SAMPLE COLLECTION: Fifty paint samples were collected by the author throughout the summer of 2009.
Small samples (ranging from 2mm to 0.5mm in diameter), were removed with a microscalpel (#11 blade), and
stored in 2 polyethylene bags which were labeled with the assigned sample number (TRC #), the element sampled
(cornice, beam, etc), sample location (north end of third beam from west), and sample description (pink flower,
glazed tin foil, etc). Each sample location was temporarily labeled with post-it arrow and photographed.
An effort was made to sample each color and metallic finish. Samples were taken from areas of existing loss or
fracture to minimize damage to the surface. Whenever possible, the same color was sampled in two different areas
to confirm that the pigments are consistent throughout the ceiling. Suspect restoration materials were also sampled
(for sample locations, see Appendix figure A-1).

2.2 ED-XRF: The elemental composition of uncast sample portions TRC-38 (metal foil) and TRC-41 (green
overpaint) were determined with an ArtTAX uXRF equipped with an energy dispersive spectrometer, which detects
elements with an atomic number of 19 (potassium) and higher. The instrument uses a molybdenum tube with a
current of 600uA, a voltage of 50kV, and a data collection time of approximately 100 seconds to target areas as

12

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

small as 70-100 microns. An integrated CCD camera captures an image of the target area for reference. Resulting
spectra were interpreted with Intax version 4.5.18.1 software.

2.3 CROSS-SECTION MICROSCOPY: All paint samples were cast in Extec Polyester Clear Resin (methyl
methacrylate monomer), and polymerized with a methyl ethyl ketone (MEK) catalyst. Once cured, they were
sanded with a rotary sander to expose the cross-section surface, and dry-polished using Micro-Mesh Inc sandpapers
with grits ranging from 1500-12000.
Mounted cross-sections were examined in the WUDPAC Paintings Conservation Laboratory with a Nikon Eclipse
80i Epi-fluorescent stereomicroscope and photographed with an attached Nikon DXM digital camera, using ACT-1
software for digital image capture in jpeg format. The samples were examined using visible light and a variety of
filter cubes with a Nikon 120 Xenon Excite lamp, including ultraviolet light (380-420nm), B-2E filter cube (450490nm), and B-2A filter cube (~546/10 nm).
The following biological stains were applied to characterize organic media:
Stain

Target Material

Solution

Filter Cube

Positive Reaction

TTC
(triphenyl tetrazolium chloride)

carbohydrates

3g in 100ml ethanol

BV-2A

Dark reddish-brown

RHOB
(Rhodamine B)

lipids

0.02% in ethanol

B-2A

Bright red fluorescence

ALEXA
(Alexafluor 488)

proteins

0.0005% in water

B-2E

Bright green fluorescence

2.4 SEM-EDS, SEM-BSE: Mounted cross-sections TRC-14 (red paint), TRC-22 (blue paint), TRC-25 (pink paint),
and TRC-27 (green paint), were analyzed for elemental composition using SEM-EDS x-ray fluorescence spot
analysis, x-ray mapping and backscattered imaging capabilities. Excess casting medium was removed with a jewelers
saw and mounted to a carbon stub with carbon tape adhesive, then coated with carbon paint up to the edge of the
cross-section to prevent charge buildup. All SEM prep materials were obtained from SPI supplies. The analyses
were carried out with a Topcon ABT-60 scanning electron microscope at an accelerating voltage of 20kV at a stage
height of 20mm with 20 sample tilt, in variable pressure mode to minimize charging. EDS data was analyzed with
a Bruker X-flash detector and microanalysis Quantax model 200 with Esprit 1.8 software.

13

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

2.5 FTIR (TRANSMISSION MODE)/ATR: FTIR was used to characterize numerous organic phases and inorganic
components found in the `adjami, paints, and varnishes. Scrapings were removed from uncast sample portions,
transferred to a diamond cell and rolled flat with a steel micro-roller to increase transparency, then analyzed with a
Thermo Scientific Nicolet 6700 FT-IR coupled with a Nicolet Continuum FT-IR microscope in transmission mode,
acquiring data with 128 scans from 4000 650cm-1 at a spectral resolution of 4cm-1. Spectra were collected with
Omnic 8.0 software and compared with various IRUG and commercial reference spectral libraries, as well as those
found in art conservation literature. ATR was used to characterize layers that could not be separated from the
greater paint stratigraphy, specifically the yellow glaze used to tone the tin foil. The instrumentation is the same as
that for FTIR, with the addition of a germanium crystal for surface analyais.

2.7 RAMAN SPECTROSCOPY: Cross-sections and bulk samples were analyzed with a Renishaw Invia Raman
spectrometer calibrated with a silicon crystal and equipped with a 785nm diode laser or a 514nm argon ion laser
operating in the range of 100 3200cm-1, with a spectral resolution of 3cm-1. Laser power (from 0.5% - 50%),
number of scans, and acquisition times (10-20seconds), were varied to collect optimal results. Spectra were obtained
with WiRE 2.0 software, and compared to online Raman reference libraries (UCL and RRUFF) as well as those
published in scientific and art conservation literature.

2.8 GC-MS: This final technique is complementary to FTIR and was used to accurately identify the proteinaceous
binding media in the blue paint (TRC-22), the lipidic binding media of the green paint (TRC-27), and the dark,
discolored varnish applied over the entire ceiling (TRC-22). Analysis was conducted with a Hewlett-Packard 6890
gas chromatogram equipped with a 5973 mass selective detector (MSD) and 7683 automatic liquid injector.
Carboxylic and methyl ester derivitives of lipidic components were volatized with 1:2 MethPrep II reagent (Alltech)
in benzene. Proteins were hydrolyzed with 50-100ul 5.5M HCl in a tightly closed vial and dried. Next, the sample
was made volatile through silylation with 100ls tertiary-butyldimethylsilyl (TBDMS). Protein and lipid samples
were analyzed with GC-MS and Agilent Technologies MSD ChemStation control software used with Winterthur

14

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

RTLMPREP method under the following conditions: inlet temperature and transfer line temperature to the MSD
(scan mode) 300C. 1uL sample volume (splitless) injected onto a 30m x 250um x 0.25um film thickness HP-5MS
column (5% phenyl methyl siloxane flow rate 1.5mL/min). The oven temperature was held at 50C for two
minutes, increased at 10C/min to 325C, and held for 10.5 minutes. Total run time was 40 minutes.

2.8 POLARIZED LIGHT MICROSCOPY: Dispersed pigment samples were mounted on a glass slide with Cargille
meltmount (refractive index 1.66). Examination was carried out in plane and cross-polarized light modes at 200x,
400x, and 1000x magnification using the Nikon Eclipse E600 POL microscope in the WUDPAC textile laboratory.

15

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

3. RESULTS
This section summarizes the results pertaining to each individual material. Please see Section 4 for further
discussion, and the Appendix for sample locations and additional data, (figures denoted A are in the Appendix).
Table 3.1 `Adjami (TRC-27[SEM-EDS], TRC-28 [CSM, FTIR])
Technique

Fig.

Data Collected

cross-section
microscopy

3.1a

SEM-EDS (xray map)

FTIR (cm-1)

3.6b

light, fluffy off-white matrix. Bluishwhite autofluorescence in UV. No stain

rxn.
Ca, S

3.1b

Material Characterization

Preliminary Interpretation

O-H stretch: 3500-3000(b);

SO42- stretch: 1100cm-1 (vs)

spectral match for calcium

sulphate dihydrate (CaSO42H2O)

N-H stretch: 3400-3200(b);

C-H stretch: ~2900
Amide triplet: 1680, 1500, 1440

spectral match hide glue (protein)

inorganic: CaSO42H2O
(gypsum)
organic: protein

Top, Figure 3.1a. Cross-section photomicrograph

of sample TRC-28, 200x, showing `adjami material
at bottom (red star).
Left, Figure 3.1b. FTIR spectrum of `adjami
scraping from TRC-28 (red), overlaid with
spectrum for gypsum (green), and hide glue
(purple).

Table 3.2 Metal foil (TRC-22[CSM, SEM-EDS], TRC-38[CSM, ED-XRF])

Technique

Fig.

Data Collected

Material Characterization

cross-section
microscopy
ED-XRF
SEM-EDS (xray map)

3.2a,
3.4e
3.2b
3.4e

150 microns thick, silver lustre. RHOB+

on underside of foil
Sn, Pb, minor Cu, (Mo source peak)
Sn in foil, Pb on underside of foil

thickness implies foil, rather than

leaf. oil mordant.
Cu possible glaze colorant
tin foil, lead drier on underside.

Preliminary Interpretation
inorganic: tin foil, lead drier
organic: oil mordant

Top, Figure 3.2a. Cross-section photomicrograph of sample TRC38, 200x, showing the tin foil layer at bottom.
Left, Figure 3.2b. ED-XRF spectrum of unmounted sample TRC38, targeting metal foil area. Peaks for Sn, Pb, and Cu are observed.

16

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

Table 3.3 Yellow glaze (TRC-38)

Technique

Fig.

Data Collected

Material Characterization

cross-section
microscopy
FTIR (cm-1)

3.3b

amber-colored in visible light, orange in

UV. No stain rxn.
O-H stretch: 3600-3000(b)
C-H stretch: 3000-2800
C=O stretch: 1700(vs)
C-C stretch: 1600
C-H bend: 1480-1300
SO42- stretch: 1100cm-1(s)

shellac

3.3a

natural resin, closest spectral

match copal.

sulfate, closest match gypsum

Preliminary Interpretation
inorganic: CaSO4 2H2O
(gypsum)
organic: natural resin, possibly
shellac. May contain an organic
dye precipitated onto gypsum
(Gettens and Stout 1942, 118)

Left, figure 3.3a: FTIR spectrum of yellow glaze over tin foil, scraping from sample TRC-38 (red), compared to reference for Zanzibar
copal (purple), and gypsum (cyan). Right, figure 3.3b: Cross-section photomicrograph of sample TRC-38. Note the orange-colored
autofluorescence of the glaze layer in ultraviolet light.

Table 3.4 Blue paint (TRC-22 [CSM, SEM-EDS, GC-MS]

Technique

Fig.

Data Collected

Material Characterization

crosssection
microscopy

3.4a,
d-e

lipids and proteins present in

binding medium

SEM-EDS
(x-ray map)
GC-MS
(mins)

3.4b,
A-2-8
3.4g

shard-like, coarsely ground blue pigment

particles; binding medium
autofluorescent, with strong RHOB+
and weak FITC+
Si, K, minor Ba, Al, As, Na, Co
amino acid derivatives: Ala(12.6),
Gly(13.6), Val(14.6), IsoLeu(15.4),
Pro(15.8), Ser(18.2), Thr(18.4), Phe(19),
Asp(18.6), Glu(20.85), Tyr(23.6)
Lipids: azelaic (20.7), palmitic (21), and
stearic acids (22.6)

potash (K) glass (SiO2), cobalt

colorant (CoO) with impurities
lack of hydroxyproline suggests
egg source. Presence of azelaic
acid suggests an aged drying oil

Preliminary Interpretation

inorganic: smalt [SiO2, K,

CoO]
organic: egg protein and
drying oil

SEM-EDS X-ray map, 250x

Top, figure 3.4a: sample TRC-22, cross-section

photomicrograph. Area analyzed with SEM-EDS highlighted in
red. Right, figure 3.4b: SEM-EDS X-ray map of sample TRC-22,

17

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

250x. Silicon (blue), potassium (pink), tin (green).

B-2A cube, FITC reaction

FITC+

G-1B cube, RHOB reaction

RHOB+

Left, Figure 3.4c: GC-MS data from sample TRC-22, layer 2 binding medium, protein analysis. The sample does not contain hydroxyproline.
Top right, figure 3.4d, bottom right, figure 3.4e: binding media analysis suggests that both lipid (RHOB) and proteinaceous (FITC)
components are present.

Table 3.5 Red paint (TRC-14[CSM, SEM-EDS], TRC-24[FTIR])

Technique

Fig.

Data Collected

Material Characterization

cross-section
microscopy

3.5a

early layer red paint, followed by

red glaze

SEM-EDS (xray map)

PLM

3.5b

two reds visible, earliest layer (1) bright

orange particles in visible light, dark red
in UV. Second red layer (2) contains
same red particles in an autofluorescent
binding medium.
layer 1: Pb, minor Fe
layer 2: minor Pb
Clumps of orange red particles, 1um,
birefringent, anomalous crosspolarization colors of orange and minor
green
Very few dark red, amorphous particles,
isotropic
layer 1: O-H stretch: 3500-3000(b)
C-H stretches: 2950, 2850 (s)
C=C stretch: 1650(s)
fingerprint region: 1170-900(b)
other: 1525(b), 1400cm-1(b)

FTIR (cm-1)

A12

Preliminary Interpretation

minium (Pb3O4)

haematite (Fe2O3)
carbohydrate, closest spectral
match psyllium seed
closest spectral match lead
tetracetate

18

inorganic: Pb3O4 (minium),

and Fe2O3 (haematite)
organic: carbohydrate with
undetermined additives

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

SEM-EDS X-ray map, 400x

Top, figure 3.5a: sample TRC-14, cross-section

photomicrograph. Area analyzed with SEM-EDS highlighted in
red.
Right, figure 3.5b: SEM-EDS x-ray map of sample TRC-14,
400x. Calcium (red) is concentrated in the gesso layer, while lead
(yellow) is concentrated in paint layer 1, with a minor presence in
layer 2.

Table 3.6 Green paint (TRC-27 [CSM, SEM-EDS, GC-MS])

Technique

Fig.

Data Collected

Material Characterization

cross-section
microscopy
SEM-EDS (xray map)
GC-MS (mins)

3.6b

thin, glaze-like, no distinct particles, no

autofluorescence in UV
Cu, Cl

Verdigris or copper resinate

no drying oil. pentachlorophenol (15.6),

dehydroabietic acid (21.8) and
7-methoxytetradehydroabietic acid (22.2)

pine resins, and 20th century

pesticide

3.6c
3.6a

copper-based green

Preliminary Interpretation

inorganic/organic:
Copper resinate

TRC-27: GC-MS results

-no drying oils present
OMe
Cl

Cl
Cl

Cl
Cl

pentachlorophenol
th

(20 -c. pesticide)

H3CO2C
dehydroabietic acid, methyl ester

(pine resin acid)

OMe
H3CO2C

SEM-EDS X-ray map, 200x

7-methoxytetradehydroabietic acid methyl ester

(pine resin acid)

Top left, Figure 3.6a: total ion chromatogram for sample TRC-27.
Drying oil was not detected, although pine resins were extant. In
addition, a 20th-century chemical pesticide was found.
Top right, Figure 3.6b: TRC-27 cross-section photomicrograph.
Note the glaze-like nature of layer 1 and its lack of autofluorescence
in UV. Are analyzed with SEM-EDS highlighted in red.
Bottom right, figure 3.6c: SEM-EDS x-ray map of TRC-27. Cu
(green) and Cl (blue) were found in the green paint, layer 1.

19

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

Table 3.7 Pink paints (TRC-25 [CSM, SEM-EDS, FITR, Raman])
Technique

Fig

Data Collected

Material Characterization

cross-section
microscopy

3.7a

Layer 2 original, Layer 4

restoration

SEM-EDS
(x-ray map)

3.7b

Layer 2: white matrix with long, red

particles with clear coating (layer 3).
Applied over metal foil (layer 1)
Layer 4: cream-colored matrix with
small blue red, and green particles.
Large, circular red and yellow particles
observed.
Layer 2: white matrix: Pb
red particles: no data
Layer 4: matrix: Zn, Ca, Ba, Pb,

FTIR (cm-1)

3.7c

Raman
Spectroscopy
(cm-1)

A-14

Layer 2: white matrix: O-H stretch:

3600-3000(b)
C-H stretch: 2925, 2853
C=O stretch: 1731
CO32-: 1401
Layer 2: red particle: N-H stretch:
3600-3100
Amide triplet: 1650, 1500, 1400
Layer 2: white matrix: 1052, red
particle: no data
Layer 4: red particle: 989, white
matrix: 1009

Layer 2: lead white with organic

red colorant
Layer 4: possibly zinc white,
chalk or gypsum fillers, barium
white/barium lake bases, lead
white, alum lake bases
lead white in drying oil

protein, closest spectral match

hide glue
2PbCO3Pb(OH)2 (basic lead
white) @ 1052 [Renishaw Raman
database]
BaSO4 (barium white) @
988(vs)[UCL]
CaSO4 (gypsum) @
1007(vs)[UCL]

Preliminary Interpretation

LAYER 2, original:
inorganic: 2PbCO3Pb(OH)2
(basic lead white)
organic: drying oil, organic
red dye with proteinaceous
fragments
LAYER 4, restoration:
inorganic: ZnO (zinc white),
2PbCO3Pb(OH)2 (lead white),
CaSO4 (gypsum), BaSO4
(barium sulphate), alum (lake
base)
organic: undermined

SEM-EDS X-ray map, 450x

Left, Figure 3.7a: TRC-25 cross-section photomicrograph. Two pink layers were observed. Layer 2 is the original pink paint. Note the
cracks and disruptions in this layer. The area chosen for SEM-EDS analysis is outlined in red.
Right, Figure 3.7b; The SEM-EDS x-ray map shows that Layer 2 is rich in lead (red). The long red particle is completely dark, indicating
its composition is exclusively organic. Layer 4 contains Pb (red), Ca (orange), Al (turquoise), Zn (yellow), and Ba (purple).

20

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

Amide I & II bands

N-H stretch
C-H stretch

Top, Figure 3.7c: red particle

excavated from sample TRC-25 for
FTIR analysis.
Left, Figure 3.7d: FTIR spectrum of
red particle (red), compared to
proteinaceous glue (purple).

Table 3.8 Green restoration paint (TRC-41)

Technique

Fig.

Data Collected

Material Characterization

Preliminary Interpretation

cross-section
microscopy

3.8b

ED-XRF
Raman
Spectroscopy
(cm-1)

3.8a

Yellow-green matrix with finely ground

pigment particles. No autofluorescence.
Applied over `adjami ornament.
Cr, Fe, Cu, Ti, Ca, minor Zn, K, Ca, Sr
123, 146(vs), 171, 178, 294, 389(s),
555(s)

Modern, synthetic binding

medium. Industrially prepared
pigments.
Cr2O3: 552(vs)[UCL]
TiO2 (anatase & rutile): 144
[Stuart 2007, 141]
Fe2O3H2O: 387 [UCL]

Inorganic: Cr2O3 (chromium

(III) oxide green), TiO2
(titanium dioxide),,Fe2O3H2O
(yellow ochre), CaSO42H2O
(gypsum)

FTIR (cm-1)

A16

C-H stretch: 3000-2850

C=O stretch: 1700(vs)
Fingerprint region: 1450, 1350
O-H stretch: 3600-3200(b)
SO42- stretch: 1125(vs)

synthetic polymer, closest

spectral match poly(ethylacrylate)

Organic: synthetic polymer,

(acrylic)

closest spectral match gypsum,

(CaSO42H2O)

Figure 3.8a. Raman spectroscopy results for the green overpaint layer in sample TRC-41 (inset, red star) Inset, figure 3.8b: TRC-41
cross-section photomicrograph. Note the green paints complete lack of autofluorescence in UV.

21

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

3.9 Restoration varnish (TRC-28 [CSM, FTIR], TRC-22 [GC-MS])

Technique

Fig.

Data Collected

Material Characterization

cross-section
microscopy

see
all

natural resin

FTIR (cm-1)

3.9a

Present in every sample, always most

recent layer applied. Brown, translucent
in visible light. Dim autofluorescence in
UV. Strong RHOB+
O-H stretch: 3600-3000(b)
C-H stretch: 3000-2800(s)
C=O stretch: 1700(vs)
fingerprint: 1450, 1375, 1200, 1110, 1050

GC-MS (mins)

3.9b

pentachlorophenol (15.5)
sandaracopimaric acid (20.7),
dehydroabietic acid (20.8),
7-oxodehydroabietic acid(22.7), 15hydroxy-7-oxodehydroabietic acid (24.2)

natural resin, closest spectral

match copal

Preliminary Interpretation

organic: natural resin, pine

source

pine resin, pesticide, no drying oil

C=O
stretch

C-H
stretch

O-H
stretch

Figure 3.9a: FTIR

spectrum of varnish taken
from sample TRC-28 (red),
compared to reference
spectrum for Zanzibar copal
mixture (purple). The data
indicates this varnish is a
natural resin. This varnish
was observed to be the most
recent layer applied in every
paint sample examined for
this study.

Figure 3.9b: Total ion

chromatogram for restoration
varnish sampled from TRC-22.
The results show an abundance of
pine resin acids, including the
methyl ester of sandaracopimaric
acid. The results also show that
pentachlorophenol, a 20th century
pesticide, is present. This chemical
was also detected in sample TRC27 (see figure 3.6a).

22

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

4. DISCUSSION
The analytical results have characterized many of the materials used to decorate, preserve, and restore the ceiling,
revealing the sophisticated techniques of Syrian craftsmen, while simultaneously shedding light on the ceilings
complicated history.
4.1 `ADJAMI: SEM-EDS x-ray mapping revealed the presence of calcium and sulfur in the `adjami (fig. 3.6b), while
FTIR further identified this material as gypsum (CaSO42H2O) in a proteinaceous binding medium, possibly a hide
glue (fig. 3.1b). The addition of glue would have lent the gypsum increased viscosity and provided the craftsman
with greater control when creating the `adjami ornaments (Wolbers May 2010, personal comment). This
composition is consistent with the research of Scharrahs (2009) and the Damascus Room `adjami (Loeblich and
Bagnall 2005), but further analysis with GC-MS is required to definitively identify the proteinaceous component as
an animal glue.
4.2 METAL FOIL: ED-XRF and SEM-EDS indicate that a foil of pure tin (Sn) was used throughout the ceiling (fig.
3.2b). No other type metallic leaf was found. SEM-EDS x-ray mapping and fluorochrome staining revealed a thin
layer of lead (Pb), and lipids (RHOB+), on the underside of the tin foil, suggesting that an oil with a lead drier was
used as a mordant (figs.A-3 & 3.4i). Tin foils were one of numerous metals used in the Nur al-Din Room
(Daskalakis-Mathews, 2000), the Dresden Damascus Room (Scharrahs, date unknown), and the Damascus Room at
Shangri La (Loeblich and Bagnall, 2005). It seems likely that tin was exclusively used on the ceiling because it is the
least expensive leaf, and various metallic effects could be imitated with tinted glazes, which were especially
convincing if viewed from the floor. Gold, being the most expensive leaf, was usually reserved for sacred
ornaments, such as passages from the Koran executed in `adjami on wall panels (Daskalakis-Matthews, 2000).
4.3 TINTED GLAZES: This analysis focused solely on the yellow glaze which lent the tin its golden appearance.
Attempts to obtain an IR spectrum for this layer within the greater cross-section stratigraphy using ATR were
unsuccessful (data not shown), but FTIR eventually revealed that the glaze is composed of a natural resin (fig. 3.3a).
This data, in combination with its orange autofluorescence in UV (fig. 3.3b), is highly characteristic for shellac.
FTIR also detected gypsum in this layer (fig. 3.3a), which could represent an organic dye precipitated onto gypsum

23

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

that could be responsible for the yellow hue (Gettens and Stout 1942, 118). Further analysis with HPLC, a
chromatographic technique sensitive to dyes, could elucidate this colorant.
4.4 BLUE PAINT: SEM-EDS analysis determined that the blue paint is made with a coarsely ground smalt (fig. 3.4b)
a potash glass tinted with cobalt oxide (SiO2, K2O,CoO). In-situ, this blue paint appears black (fig. A-1), which
initially suggested that pigment deterioration was extensive. Smalt has been documented to degrade when bound in
oil, as the alkaline potassium components are leached from the glass network by the acidic media (Spring 2005, 1).
However, the ceilings smalt was observed to retain much of its blue hue in cross-section (fig. 3.4a), and x-ray
microanalysis in the SEM was unable to identify any distinct variation between potassium content in particles at the
top and bottom of the layer (data not shown). At this time, the present color shift in the blue paint does not appear
to result from any inherent vice in the paint itself, but likely results from the dark restoration varnish applied to
the entire ceiling (see Section 4.10 for additional discussion).
The autofluorescent binding medium for the smalt stained positively for proteins and oils using fluorochrome stains
(fig. 3.4d-e). The medium was further identified as an egg protein via GC-MS, which revealed a range of amino
acids with the distinct absence of hydroxyproline, the principal amino acid in collagen (fig. 3.4c). It should be noted
that the peaks for azelaic, palmitic, and stearic acids seen in the chromatograph are not reliable markers for drying
oils. In fact, lipidic analysis with GC-MS on another portion of the same smalt sample (TRC-22), determined there
were no drying oils present (fig. 3.9b). While numerous `adjami rooms in Western collections report the use of smalt
in animal glue (Scharrahs, various), the ELISA determined that egg proteinwas used to bind smalt in the
Metropolitans Nur al-Din Room (Arslanoglu 2009). An emulsion of protein and oil was suggested with FTIR in a
green paint from Shangri Las Damascus Room (Loeblich and Bagnall, 2005, 32-34), although this was not analyzed
with GC-MS.
4.5 GREEN PAINT: The green paint was identified as copper resinate, a brilliant green made by dissolving verdigris
(Cu(C2H3O2)2 2Cu(OH)2) in heated pine resins. Verdigris is a complex mixture of basic copper acetates with
copper chlorides and/or copper carbonates (Kuhn 1970, 12), which accounts for the copper and chlorine identified
via SEM-EDS x-ray mapping (fig. 3.6c). In cross-section, the glaze-like nature of the green and its complete lack of
autofluorescence are consistent with the properties of copper resinate (fig. 3.6b), and this was further supported by

24

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

GC-MS analysis, which detected the methyl esters of pine resin acids, but failed to find any drying oil in the sample
(fig. 3.6a). FTIR and Raman spectroscopy were unable to identify copper resinates, verdigris, or any other copperchloride greens reported in Eastern artworks, such as atacamite or paratacamite minerals (Lazzarini and
Schwartzbaum 1985). Although copper-based greens, especially verdigris, are reported in other `adjami rooms
(Scharrahs, date unknown), no sources known to the author have specifically reported the use of copper resinates in
a Damascene interior.
4.6 RED PAINT: SEM-EDS and PLM revealed that the red paint is composed of red lead (minium), and a very
small amount of iron oxide (figs. A9-A11). Cross-section microscopy suggests that two layers were used to build up
the red: first, a pigment-rich layer followed by a red glaze composed of an autofluorescent binding medium, most
likely to impart a glossy surface to the red details (fig. 3.5a). A similar technique was found in the Aleppo Room in
Berlin, where reds were applied in three layers starting with a layer of minium, followed by a thin layer of vermillion,
and finally a natural resin (Scharrahs, date unknown). FTIR analysis of the red paint suggests that a mixture of
binding media was used, the closest spectral matches being Psyllium seed: a carbohydrate material, and lead
tetracetate: a metal drier for oil vehicles (fig. A-12). This complex mixture could be further identified with GC-MS.
4.7 PINK PAINT(S): Two pink paint layers are visible in cross-section (fig. 3.7a). The original pink layer (2) is a
dense, white matrix containing unusually long, slim red particles (see also fig. 3.7c). The second pink layer (4)
appears to have been applied well after the ceilings completion, as it can be seen to flow into pre-existing cracks in
the original pink. The SEM-EDS x-ray map identified lead (Pb) in the original pink paint, but the long red particles
were completely dark, indicating that their compositions are exclusively organic (fig. 3.7b). Raman spectroscopy of
the white matrix yielded a distinct band at 1057cm-1, characteristic for 2PbCO3Pb(OH)2, (basic lead white) (fig. A14), while FTIR identified the binding medium as a drying oil (fig. A-13). However, no conclusive data was obtained
for the red particles with Raman, despite numerous attempts on both mounted and unmounted samples. Finally, a
red particle was excavated out of the paint film and a scraping was obtained for FTIR analysis. The results indicated
that these particles are proteinaceous (fig. 3.7d), providing two possible explanations for their identity. The first
theory suggests that these are small bits of wool or silk onto which an organic red dye was precipitated. This process
is described in a 16th century treatise by Sdiq Bek, a Persian court painter who describes the production of red lake

25

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

by heating stick-lac in hot water to extract the organic dye, which is then precipitated onto sdeh - small scraps of
rag or cloth (Bek, c.16th c., translation date unknown). Presumably, these tiny textile fragments were ground directly
into the white paint, or could be wet with an aqueous medium to release the lake which imparted a pink color to the
white paint. A second theory suggests that the red particles are unstrained fragments of cochineal or kermes insects
used to make a red lake. Since arthropod exoskeletons are composed of chitin in a proteinaceous matrix, the FTIR
spectrum supports this theory. To investigate further, the author ground dried cochineal insects into lead white with
oil and examined the results in cross-section. The color and morphology of the cochineal fragments provide
compelling evidence that the Turkish Room red particles are indeed the fragments of cochineal or kermes insects
trapped in a lead white matrix (fig. A-15). However, the analysis was unable to identify precisely what is responsible
for the overall pink color of the paint, since the insect fragments made a gritty paint with a purple-gray tone that
would have been unsuitable for painting. A liquid chromatographic method, such as HPLC, is recommended to
identify the organic red in the pink paint and additional reconstructions are recommended to investigate the sdeh
theory.
The second pink paint layer (fig. 3.7a, layer 4) was found to contain zinc, which suggests that ZnO (zinc white) is
present, a pigment that was not commercially available until c.1835 (Gettens and Stout 1942, 177). This data
suggests that layer 4 is a restoration paint that could have been applied in Damascus.
4.8 PESTICIDE: The presence of pentachlorophenol, an industrial strength pesticide, was discovered via GC-MS in
two samples (figs. 3.9b & 3.6a). PCP was introduced in the 1930s and became illegal in the United States in 1980,
due to its extreme toxicity (PCP Wikipedia page 2010). Therefore, this chemical must have been applied to the
ceiling some time after its arrival in the United States, although the analysis cannot determine an exact date. It is
interesting to note although the Turkish Room wall panels were severely damaged by a termite infestation in 1983,
very little damage was observed on the ceiling.
4.9 GREEN OVERPAINT: FTIR characterized the binding medium for the olive colored touch-up paint as an
acrylate resin (fig. A-16), which was not commercially available as a paint medium until c.1940 (Lerner 2004, 3).
Post-historic pigments including chromium oxide green (earliest known availability as a pigment c.1862) and
titanium dioxide (introduced 1914), were identified via Raman spectroscopy (fig. 3.8a). This data suggests these

26

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

paints were applied at least a decade after the ceiling had arrived in the United States, although it has been generally
assumed that these touch ups were carried out by Duke and her staff at Shangri La c.1980 (Travers and Barnes,
2009).
4.10 VARNISH: Cross-section microscopy revealed a thick layer of varnish over all of the decorative surfaces, which
FTIR identified as a natural resin, the closest spectral match being a copal (fig. 3.9a), while GC-MS detected
multiple pine resin acids including sandaracopimaric acid (fig. 3.9b), a resin acid associated with copal and sandarac
varnishes (Stuart 2007, 121). Both resins are described as dark varnishes that become darker with age (Gettens
and Stout 1942, 15, 59), which provides an explanation for the overall brown tone of the ceiling. In addition, GCMS revealed negligible amounts of palmitic and stearic acids, suggesting that this was not an oleo-resin but a wholly
spirit varnish. Tragically, this spirit varnish has irreversibly solubilized the shellac which lent the tin foil its colored
lustre. This effect is clearly illustrated by sample TRC-28 (fig. A-17), which shows the shellac being actively drawn
up into the later varnish. It is unclear exactly when this coating was applied, although its appearance on top of the
green synthetic touch up paint (fig. 3.8b), suggests that it could have been applied at Shangri La. However, none
of Doris Dukes former employees recollect varnishing the ceiling as part of the restoration effort (Travers and
Barnes 2009), and there is no mention of varnishing the ceiling in the Turkish Room archives. Additional samples
should be collected from overpainted areas to clarify the ceilings restoration history.

5. CONCLUSIONS
This study achieved its primary goal to identify many of the materials used to create the Turkish Room ceiling, and
elucidate the sophisticated techniques used by 18th century Damascene artisans to bring these architectural surfaces
to life. The intricate `adjami ornaments are composed of gypsum in animal glue, coated with tin foil and shellacked
to imitate gold. Paints include a blue composed of smalt bound in egg, copper resinate greens, minium and iron
oxide reds, and pinks made with white lead and an organic red lake in a drying oil. A digital reconstruction based on
the analytical results (fig. A-18) clarifies these findings and illustrates the ceilings original function- to create an
atmosphere of dazzling color and opulence fit for an aristocratic Damascene home.

27

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

The analysis also found that the ceiling retains a thick layer of non-original spirit varnish that has darkened with age.
This coating distorts the original color scheme and has irreversibly solubilized the original shellac glazes which lent
the tin leaf its golden lustre. Other non-original materials include a pink overpaint that could have been applied in
Damascus, as well as a chemical pesticide and acrylic paints applied when the ceiling was in the United States.
Additional research is warranted to further explore the identity of the long red particles in the pink paint, the use of
a yellow colorant in the golden shellac coating, and the establishment of a time frame for the acrylic overpaint and
the copal/sandarac varnish to identify exactly which activities were carried out by Duke and her staff at Shangri La.

6. ACKNOWLEDGEMENTS
I would like to extend my sincere thanks to all of the people who helped me complete this project, especially the
SRAL scientists: Dr. Jennifer Mass, my project supervisor; Dr. Joe Weber; Dr. Chris Petersen; and especially
Catherine Matsen for helping me get an early start in Fall 2009; Mary McGinn, who suggested I use the ceiling for
my technical study in the first place; Richard Wolbers, my major supervisor; Mecka Baumeister, Beth Edelstein, and
everyone on the Metropolitan Museum of Arts Nur al-Din Room conservation team; Anke Scharrahs, conservator
and scholar of `adjami interiors; Melanie Gifford for her assistance with PLM, Natasha Loeblich for suggesting the
cochineal exoskeleton theory; the Doris Duke Foundation for Islamic Art and Shangri Las wonderful staff,
especially Deborah Pope, Sharon Littlefield, and Maja Clark; and finally, all of my WUDPAC classmates, especially
LeeAnn Barnes-Gordon, with whom I shared an entire wonderful summer beneath the Turkish Room ceiling.

7. REFERENCES
Arslanoglu, J. and J. Schultz. 2009. Immunology and art: using antibody-based techniques to identify proteins and
gums in binding media and adhesives. Metropolitan Museum of Art Bulletin: 40-48.
Burgio, L., R. Clark, et al. 2008. Pigment analysis by Raman spectroscopy of the non-figurative illumination in 16thto 18th-century Islamic manuscripts. Journal of Raman Spectroscopy 39: 1482-1493.
Cennini, C. 15th c. The craftmans handbook. Trans. Daniel Thompson. New York: Dover Publications, Inc.
Sister Daniilia, S. Sotiropoulou, D. Bikiaris, C. Salpistis, G. Karagiannis, Y. Chryssoulakis, B. Price, J. Carlson. 2000.
Panselinos Byzantine wall paintings in the Protaton church, Mount Athos, Greece: a technical examination. Journal
of Cultural Heritage 1: 91-110.

28

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

Daskalakis-Mathews, A. 1997. A room of splendor and generosity from Ottoman Damascus. Metropolitan Museum
Journal 32: 111-139.
Eastaugh, N., V. Walsh, T. Chaplin, and R. Siddall. 2008. Pigment compendium: a dictionary and optical microscopy of
historical pigments. Oxford, Butterworth-Heinemann.
Evans, J. 2008. Sacrifice of Isaac by Antionio di Donnino del Mazziere: technical analysis and conservation
treatment. Association for North American Programs in the Conservation of Cultural Property annual conference.
Unpublished presentation. New York University Conservation Center, Institute of Fine Arts.
Headley, B. and L. Orsini. 2007. The Damascus Room: conservation and documentation, phase III. Summer work
project report, Winterthur / University of Delaware Program in Art Conservation.
Gettens, R., and G. Stout. 1942. Painting materials: a short encyclopedia. New York: Dover Publications, Inc.
Keenan, B. 2000. Damascus: hidden treasures of the old city. London: Thames and Hudson, Ltd.
Kuhn, H. 1970. Verdigris and copper resinate. Studies in Conservation 15, 12-36.
Lazzarini, L., and P. Schwartzbaum. 1985. The technical examination and restoration of the paintings of the dome
of the Al Aqsa mosque, Jerusalem. Studies in Conservation 30 (3): 129-135.
Lerner, T. 2004. Analysis of modern paints. Getty Conservation Institute.
Littlefield, S. 1999. Transcript of personal interview with Jin de Silva, conducted October 1999.
Loeblich, N. and A. Bagnall. 2005. The Damascus Room: conservation and documentation, phase II. Summer work
project report, Winterthur/University of Delaware Program in Art Conservation.
Loeblich, N. and C. Matsen. 2006. Cross-Section microscopy report: Morning Room, the Breakers. Unpublished
report, Winterthur / University of Delaware Program in Art Conservation.
Matsen, C. 2006. The Corbit-Sharp house at Odessa, Delaware: finishes analysis and interpretation of four interior
rooms. In Paint Research in Building Conservation, ed. L. Bregnhoi et al. London: Archetype: 21-30.
Nadolny, J. 2006. All thats burnished isnt bole. Reflections on Medieval water gilding part I: early Medieval to
1300. In Medieval painting in northern Europe: techniques, analysis, art history, ed. J. Nadolny. London: Archetype. 148-162.
Paccard, A. 1980. Traditional Islamic craft in Moroccan architecture: tome 2. Saint-Jorioz, France: Edtions Atelier 74.
Purinton, N. and M. Watters. 1991. A study of the materials used by medieval Persian painters. Journal of the American
Institute for Conservation 30 (2): 125-144.
Scharrahs, A. 2009. About the colour scheme and painting technique of Damascene wooden interiors- the ajami
rooms in the houses Bayt al- Aqqad and Bayt al- Hawraniya. Unpublished typescript.
Scharrahs, A. date unknown. Ajami rooms- polychrome wooden interior decorations from Syria of the 17th to the
19th centuries: a view into art technology and conservation problems. Unpublished typescript.
Spring, M., C. Ricci, and D. Peggie. 2008. ATR-FTIR imaging for the analysis of organic materials in paint crosssections: case studies on paint samples from the National Gallery, London. Journal of Analytical and Bioanalytical
Chemistry. 392: 37-45.

29

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

Stuart, B. 2007. Analytical Techniques in Materials Conservation. West Sussex: John Wiley & Sons, Ltd.
Travers, K. and L. Barnes. 2009. Documentation and consolidation of the Turkish Room ceiling at Shangri La.
Summer work project report, Winterthur / University of Delaware Program in Art Conservation.
Wolbers, R. and G. Landrey. The use of direct reactive fluorescent dyes for the characterization of binding media in
cross sectional examinations. AIC Preprints. American Institute for Conservation 15th Annual Meeting, Vancouver.
Washington, D.C.: AIC.

BIBLIOGRAPHY
Littlefield, S. date unknown. Summary of the components of the Turkish Rooms. Unpublished typescript. Shangri
La, Honolulu, HI.
Littlefield, S. 2008. The Turkish and Baby Turkish Rooms at Shangri La. Unpublished typescript. Shangri La,
Honolulu, HI.
Littlefield, S. 2002. Doris Dukes Shangri La. Honolulu: Doris Duke Foundation for Islamic Art.
Mansfield, S. 1992. The Richest Girl in the World: The Extravagant Life and Fast Times of Doris Duke. New York: Pinnacle
Books.
Mortensen, P., eds. 2005. Bayt al-Aqqad: the history and restoration of a house in Damascus. Proceedings of the Danish
Institute in Damascus IV. Denmark: Aarhus University Press.
Prial, F. date unknown. 2 old Syrian rooms go on display. New York Times: 46.
Scharrahs, A. 2003. Das Dresdner Damaskus-zimmer. English translation of exhibit publication from Staatliches
Museum fur Volkerkunde, Dresden.

30

ATRC 673- TURKISH ROOM CEILING TECHNICAL STUDY

APPENDIX
SAMPLE LOCATIONS (1)
TRC-22 X-RAY MAPS & XRF SPECTRA (2)
TRC-14 X-RAY MAPS (2)
TRC-24 FTIR SPECTRA (3)
TRC-25 FTIR SPECTRA (3)
TRC-25 TABLE OF RAMAN RESULTS (4)
COCHINEAL IN LEAD WHITE RECONSTRUCTION (4)
TRC-41 FTIR SPECTRUM (5)
TRC-28 CROSS-SECTION PHOTOMICROGRAPHS (5)
DIGITAL RECONSTRUCTIONS (6)

31

APPENDIX TURKISH ROOM CEILING TECHNICAL STUDY

Figure A-1. Sample locations

APPENDIX TURKISH ROOM CEILING TECHNICAL STUDY

Figures A-2-8. TRC-22 XRF spectra and X-ray maps (SEM-EDS)

Figure A-3. Pb x-ray map

Figure A-2. TRC-22, X-ray spectrum at 250x

Fig. A-5. As x-ray map

Figure A-4. Co x-ray map

Fig.A-6. Ba x-ray map

Fig.A-7. Al x-ray map

Fig.A-8. Na x-ray map

Figures A-9-11. TRC-14 x-ray maps (SEM-EDS)

Fig. A-9. Ca x-ray map

Fig. A-10. Pb x-ray map

Fig. A-11. Fe x-ray map

APPENDIX TURKISH ROOM CEILING TECHNICAL STUDY

Figure A-12. FTIR spectrum of sample TRC-24

Figure A-13. FTIR spectrum of sample TRC-25 original pink paint

APPENDIX TURKISH ROOM CEILING TECHNICAL STUDY

Figure A-14. TRC-25 Raman results (Renishaw Raman 1000, 785nm laser)
Raman
target
R1
R2

Laser power
(LP) and time
(s)
5% LP, 10s
10% LP, 10s
50% LP, 10s

1009 cm-

50% LP, 20s

1009 cm-

10% LP, 10s

1052 cm-

Peaks
Observed

Match (UCL Raman

Spectroscopic Library)

989 cm-1

BaSO4 (barium
white) @ 988(vs)
CaSO4 (gypsum) @
1007(vs)

1
1

R3

R4

0.5% LP, 10s

1% LP, 10s
5% LP, 10s

no data
no data
1086cm-1

10% LP, 10s

50% LP, 10s

no data
oversatur
ation
no data
oversatur
ation

5% LP, 20s
10% LP, 20s

2PbCO3 Pb(OH)2
(basic lead white) @
1050 (vs)
none
none
Chalk (CaCO3), from
dust on sample
none
none
none
none

Figures A-15 a-b. Reconstruction pink paint compared to TRC pink paint

Figure A-15a. Sample TRC-38, visible light, 200x

Figure A-15b. Cochineal ground in lead white

and oil, visible light, 400x

APPENDIX TURKISH ROOM CEILING TECHNICAL STUDY

Figure A-16. FTIR spectrum of TRC-41 green overpaint

The data suggests the overpaint is composed of an acrylic medium with a gypsum filler.

Figure A-17a-b. Later varnish solubilizing original shellac

Figure A-17a. Sample TRC-28 resanded. Visible

light, 100x

Figure A-17b. Sample TRC-28 resanded.

Ultraviolet light, 100x. The arrows indicate the
globs of original shellac being solubilized and
drawn up into the later varnish.

APPENDIX TURKISH ROOM CEILING TECHNICAL STUDY

Figure A-18a. Digital reconstruction based on analytical results

This portion of the NE cornice was reconstructed as it was the origin for most of the analyzed samples.

Figure A-18b. Digital reconstruction magnified

This image was made using Adobe Photoshop

APPENDIX TURKISH ROOM CEILING TECHNICAL STUDY