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Characterization of 17th Century Mughal tile glazes from Shahdara Complex,

Lahore-Pakistan

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DOI: 10.1016/j.culher.2012.03.007

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 Journal of Cultural Heritage 14 (2013) 174–179

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Case study

Characterization of 17th Century Mughal tile glazes from Shahdara Complex,

Lahore-Pakistan
Saima Gulzar a,∗,b , Marie Wörle c , Jean-Pierre Burg d , Muhammad Nawaz Chaudhry a , Edith Joseph e ,
Eric Reusser f
a
College of Earth and Environmental Sciences, University of the Punjab-Lahore 54590, Pakistan
b
Swiss Federal Institute of Technology Zurich, Geological Institute, NO E 17, Switzerland
c
Head Conservation Research, Swiss National Museum, Sammlungszentrum, Lindenmoostrasse 1, Switzerland
d
Swiss Federal Institute of Technology Zurich, Geological Institute, NO E 67, Sonneggstrasse 5, 8092 Zurich, Switzerland
e
Marie Curie-Intra European Fellow, Swiss National Museum, Sammlungszentrum, Lindenmoostrasse 1, 8910 Affoltern a. Albis, Switzerland
f
Swiss Federal Institute of Technology Zurich, Institute for Geochemistry and Petrology, NW E 85, Clausiusstrasse 25, 8092 Zurich, Switzerland

a r t i c l e i n f o a b s t r a c t

Article history: The glazed tile decorative art was one of the widely used ornamental techniques for the monumental
Received 23 August 2011 buildings during the Mughal period, in Pakistan. Coloured tile samples from Jahangir tomb were analyzed
Accepted 19 March 2012 to know the glaze composition and to identify the colouring phases used at that time. The study was
Available online 3 May 2012
performed using light microscopy (OM), scanning electron microscopy equipped with energy dispersive
X-ray analyzer (SEM-EDS), Raman spectroscopy (RS) and electron microprobe analysis (EMPA). These
Keywords: complementary analytical techniques allowed characterizing the samples as alkali glazes made from
Glazed tiles
plant ashes. The results indicated the use of lead-tin yellow type II for yellow glazes, cobalt and copper
Pakistan
Microscopy
for blue glazes, mixtures of yellow and blue glazes for the green glazes, manganese for purple glazes, and
SEM a transparent glaze layer for white glazes.
Raman © 2012 Elsevier Masson SAS. All rights reserved.
Electron microprobe
Glaze
Colourants

1. Introduction ornamental techniques for the monumental buildings of that par-

Pakistan possesses rich and diverse cultural heritage composed
of a long and continuous history starting since the Stone Age. The
built heritage reflects the materials, tools and construction tech-
niques of any particular era. Studies of these historical monuments
provide the ways and means to restore these landmarks of history.
Unfortunately, conservation of heritage is not given much priority
in Pakistan where it is considered as a resource intensive activity
rather than part of development. The lack of state interest, funds,
information and research on historic materials and techniques are
the major causes of inadequate conservation of the heritage sites
in Pakistan.
The glazed tile decoration technique emerged as a unique
art of its own kind during the Mughal period (1526–1857 A.D.)
in the subcontinent and it became one of the widely used
∗ Corresponding author. Tel.: +92 42 35 85 58 27; fax: +92 42 35 83 18 66.
E-mail addresses: saimagulzar@yahoo.com, saima.gulzar@erdw.ethz.ch (S.
Gulzar), marie.woerle@snm.admin.ch (M. Wörle), jean-pierre.burg@erdw.ethz.ch
(J.-P. Burg), muhammadnawazchaudhry@yahoo.com (M.N. Chaudhry),
edith.joseph@snm.admin.ch (E. Joseph), eric.reusser@erdw.ethz.ch (E. Reusser).
ticular era. But this particular decorative technique is now almost
extinct in Pakistan due to the lack of information on its materi-
als and manufacturing technology. Although Mughal architecture
has been explored with the available limited resources, many of
the ornamental techniques have yet to be identified so far. The
glazed tile decorative art is one of these, and the lack of knowl-
edge on the subject often leads to failure in restoration attempts
as also observed in ongoing conservation-restoration projects on
world heritage sites in Pakistan.
The 17th century tomb of Jahangir built during the reign of
Emperor Shah Jahan is one of the majestic monuments in the Shah-
dara complex. The tomb was built with a brick and lime mortar
masonry core and with red sandstone and white marble inlays
depicting characteristic features of the Mughal architecture. The
interior of the building was decorated with glazed tiles following
the popular scheme of floral patterns used for decorating buildings
of Mughal era. It was made with two different blues in combination
with white and purple-coloured flowers on a deep mustard yellow
ground and a surrounding green border (Fig. 1).
A systematic examination of the colour glazes from different
periods has already been performed in different parts of the world.
However, there is a lack of scientific research and analysis of the

1296-2074/$ – see front matter © 2012 Elsevier Masson SAS. All rights reserved.
doi:10.1016/j.culher.2012.03.007
 S. Gulzar et al. / Journal of Cultural Heritage 14 (2013) 174–179
Fig. 1. Jahangir Tomb: wall showing the glaze sampling details.
Mughal decorative arts especially for the colour glazes in Pakistan.
The results presented in this paper are the first concerning the glaze
composition and the colouring phases used for the production of
the Mughal period glazes in Pakistan.
2. Research aims
The aim of this work is to present the preliminary scientific
examination of the colouring phases in glazed tile specimens
collected from the monumental structures of the 17th century
Mughal Shahdara Complex in Lahore-Pakistan. This pioneer study
could also shed light on the manufacturing technology of the
time. The identification methodology integrates the results from
optical microscopy, scanning electron microscopy with energy dis-
persive X-ray spectroscopy (SEM-EDS), Raman spectroscopy and
electron microprobe (EMPA). These analyses are important for the
conservation-restoration of the glazed tiles technology from the
Mughal architecture, which are rapidly deteriorating. The project
was conducted in collaboration with several institutions: the Col-
lege of Earth and Environmental Sciences of the University of the
Punjab-Lahore (Pakistan), the Department of Earth Sciences of the
Swiss Federal Institute of Technology, ETH-Zurich (Switzerland)
and the conservation research laboratory of the Collections Center
from the Swiss National Museum (Switzerland).
3. Historical background
The Mughal decorative art of glazed tiling evolved over cen-
turies. It originated from simple painted bricks to terracotta, baked
clay tiles and finally to coloured glazed tiles. The earliest glazed
tiles were discovered near Thebes in Egypt (from pre-dynastic
period before 4777 B.C.) and from Mesopotamia, where the art
of glazed tiling was particularly flourishing from ancient times
[1,2,3,4]. The ancient civilizations of Babylonia and Assyria in
Mesopotamia developed polychrome brickwork, which was then
perpetrated until the Persian period (539–331 B.C.) and character-
ized by abundant details in the decorations [3,5]. The art of glazed
tile decorations traveled to the Indian subcontinent during the early
centuries of the Christian era but was confined to Sindh (Pakistan)
and Bengal (India) [2,3,6]. The Arabs adopted this traditional art
175
from Iran after Islamic conquest of Persia and used it later to embel-
lish their buildings while spreading it all over the Islamic world.
Glazed tiles became an essential component of architectural
construction after the 11th century in Iran and developed as the
characteristic feature of Muslim architecture. In 1167 to 1168 A.D.,
Kashan (Iran) flourished as the manufacturing center of the most
beautiful glazed “Kashani Tiles”. The Iran production spanned a long
time period from the 13th to the 15th century. The technique spread
to Egypt, Syria, and Central Asia during the 14th and 15th centuries.
The art of glazed tiles was introduced to the Indian subcontinent
by Muslims coming from Timurid Central Asia (1360–1500 A.D.)
[6,7,8].
The development of these decorations started in the subconti-
nent with the advent of the Mughal rule in 1526 A.D [3,6,7]. Glazed
tile decorations were systematically employed during the reign of
Emperor Akbar (1556–1605 A.D.). His son, Jahangir (1605–1627
A.D.), adopted glazed tiles for ornamentation and murals such as on
the pictural wall of Lahore Fort [3,6,7]. These decorations flourished
and reached a peak during the Shah Jahan’s period (1628–1658
A.D.). The monuments constructed during this period are unique
for to the fact that the glazed tiles were of two types, locally made
stonepaste body, at variance from the imported Iranian glazed tiles
based on terracotta, which were also diffused in other parts of the
world [7].
4. Analytical techniques
The number of samples was limited to avoid further damaging
to monuments of historical value. Sampling was carried out under
the supervision of the conservators in charge. Seven samples (one
or two samples for each colour) were taken from the western wall
of Jahangir’s tomb with respect to the main entrance (Fig. 1). The
samples were mounted in polyester resin (technovit 200LC), cross-
sectioned and polished with conventional methods using silicon
carbide card with successive grids (from 120–1000 as required).
Optical microscopy was performed to identify the different lay-
ers of the samples under both visible and ultraviolet lights. The
resulting stratigraphy revealed occasional restoration interven-
tions together with textural and structural information on the
manufacturing technique of these glazes. The cross sections were
observed in dark field in an optical Axioplan Zeiss microscope
and Epiplan-Neoflaur objectives from 2,5 × to 50 × magnification.
The photomicrographs were obtained with the attached Axiocam
Zeiss camera. In some cases, the observations under ultraviolet
light allowed distinguishing between the fused compounds of the
coloured layer. The cross sections were then analyzed by SEM-EDS,
after carbon sputtering. The instrument is a JEOL JSM-6390LA scan-
ning electron microscope with an energy dispersive X-ray analyzer
working in the accelerating voltage range of 0 to 10 kV. The semi-
quantitative analysis of elemental composition was also calculated
with the JED-2300 Analysis Station software, at an acceleration
voltage of 15 kV and an acquisition time greater than 50 s.
Specific areas of the cross-sectioned samples were also ana-
lyzed with a JEOL Electron Microprobe Analyzer JXA 8200 equipped
with a secondary electron (SE) and a back scattered electron (BSE)-
detector, 5 wavelength dispersive X-ray spectrometers (WDS) and
an energy dispersive X-ray spectrometer (EDS) with an accelerating
voltage from 0.2 to 40 kV, a probe current range from 10−12 to 10−5
A and a stage speed maximum of 5 mm/s. This allowed an accurate
and quantitative analysis of the glaze layer.
The Raman spectra on the cross section were generated using a
Labram Aramis Raman spectrometer (Horiba Jobin Yvon) equipped
with a Peltier cooled CCD (1024 × 256 pixels), fully automated
grating system (600–1800g/mm), edge filter and laser selection
between a laser diode at 785 nm, a He/Ne laser at 632.8 nm and a
176 S. Gulzar et al. / Journal of Cultural Heritage 14 (2013) 174–179

Fig. 2. Photomicrographs of cross-sectioned samples (original magnification 100 ×): (a) Yellow glaze S32Y, (b) dark blue glaze S52B, (c) light blue glaze S76B, (d) green glaze
S45G, (e) purple glaze S44P and (f) white glaze S44 W.

Nd:Y Ampere (A) laser at 532 nm. The scattering light was collected
on different spots of the glaze layers through 10 ×, 50 × and100 ×
Olympus objectives; at least four different points were measured
with five accumulations for each point.
5. Results
Under optical microscopy and SEM observations, all samples
(locally known as Kashi tiles) showed a glassy glaze layer (Fig. 2)
of uniform thickness (100–200 ␮m) spread on a stonepaste body
mainly composed of silica but under further investigation.
The preparation of the colour glazes, employing heating and
fusing, was a lengthy process consisting of a series of operations.
Sintering, one of the major processes was to make easily fusible
glass by melting powdered siliceous sand with sodium carbonate
in the Mughal period [9,10]. The mixture was then fused with
reduced metallic oxides obtained from local raw materials in
special furnaces. Afterwards, glazes were applied on the silica-rich
stonepaste body [2,3,6,9,10].
The studied glazes typically yield high soda contents rang-
ing from 10 to 15% [11,12]. The glazes also showed appreciable
amounts of lime, potash and magnesia (Table 1), suggesting the uti-
lization of plant ashes to make the glaze suspensions [13]. The lime
content ranged from 2 to 3.5%, potash from 2 to 6.7% and magnesia
is about 4% in all analyzed glazes [14,15].
5.1. Yellow glazes
Optical microscopy examination of sample S32Y showed a
single yellow layer (100–150 ␮m thick) containing irregularly dis-
tributed yellow and few orange particles (Fig. 2a). Bubbles trapped
within the glaze layer were found in significant amount. They can
 S. Gulzar et al. / Journal of Cultural Heritage 14 (2013) 174–179 177

Table 1
Glaze composition determined by Electron Microprobe Analysis (EPMA).

Sample Color SiO2 Al2 O3 Na2 O K2 O MgO FeO CaO PbO SnO2 CoO CuO MnO ZnO Cr2 O3 SO3 P2O5

S32Y Yellow 59.87 1.27 12.22 2.41 3.11 0.37 2.35 11.36 2.17 – – – 0.23 – 0.03 0.24
S82Y Yellow 58.87 1.23 10.97 3.01 2.77 0.21 3.12 13.78 2.67 – – – 0.17 – 0.01 0.34
S52B D-blue 71.75 1.21 11.25 3.31 2.51 2.30 3.52 – – 0.61 0.49 – – – 0.17 0.25
S76B Blue 72.23 1.33 11.13 3.07 2.71 1.91 3.18 – – 0.22 0.19 – – – 0.17 0.19
S45G Green 53.26 1.98 12.27 2.47 2.17 0.31 2.27 12.73 2.32 0.07 2.37 – 0.32 – 0.27
S44P Purple 69.57 1.36 14.97 6.61 2.32 0.68 2.27 – – – – 1.17 – 0.04 0.17 0.21
S44W White 72.30 1.37 10.38 5.31 2.56 1.97 2.05 – – – – – – – 0.09 0.27

(–): oxides present below the instrumental detection limit.

be attributed to the decomposition of calcium carbonate, which
released carbon dioxide during the firing and fusion process. This
observation is in accordance with the manufacturing technology of
such glazed tiles as reported in literature [15]. The electron micro-
probe analysis (EPMA, Table 1) showed lead and tin as the primary
colouring agents probably used as lead-tin yellow with associated
zinc content. The average 0.2% zinc oxide probably comes from
impurities of the lead oxide.
The lead-tin yellow pigments were widely studied by Kuhn
(1968) and Clark et al. (1995). Two types were defined: type I
(PbSnO4 ), and type II (PbSn1-x Six O3 ). Both types were used as
paint pigments in Europe before the 18th century but the type II
was mainly associated with the manufacturing of glass and glazes
[16,17].
We cannot ascertain the use of lead-tin yellow type I rather
than type II. In fact, type II is obtained by heating type I at around
950 ◦ C (Pb2SnO4 + SiO2 → PbSn1-x Six O3 , at T = 800–950 ◦ C) [16,17]
which is the same range of temperatures used for fusing glazes
during the Mughal period as documented in ancient text [18–20].
In support, the Raman spectra of yellow and orange particles
(Fig. 3) were compared with the lead-tin type I and type II (both
pigments synthesized at the Doerner Institut in München). The yel-
low and orange particles showed intense bands at 141 cm−1 and
broad scattering bands at 332 cm−1 /337 cm−1 with weak bands
at 445 cm−1 /432 cm−1 /476 cm−1 which can be attributed to the
lead-tin yellow type II [21–23]. Additionally, orange particles spec-
trum showed other bands at 115 cm−1 , 161 cm−1 , 533 cm−1 and
648 cm−1 that can be attributed to differential heating and fusing
process and will be further investigated.
One can assume that craftsmen (Kashigars) of Mughal era inten-
tionally manufactured the lead-tin yellow type II through the fusion
of reduced metallic oxides (Pb and Sn) with a silica glass (SiO2 ) to
obtain an intense yellow hue at 900 to 950 ◦ C (locally known as
zarda) different from the lemon yellow hue of lead-tin yellow type
I.
Further analyses should be carried out in order to distinguish
between the two types, specify the glazes starting either from lead-
tin yellow type I or II and study the different fusion processes in
relation with different temperatures.
5.2. Blue glazes
The blue glaze samples (S52B, S76B) showed a homogeneous,
about 200 ␮m thick glaze layer with few, sporadically distributed
red particles (iron oxide) in the optical microscopy of cross-
sectioned samples (Fig. 2b and c). Two blue glazes were different
in tonality as S52B (Fig. 2b) is darker than S76B (Fig. 2c). The EPMA
analysis (Table 1) revealed the presence of cobalt and copper. His-
torically cobalt was used in glazes to give enriched blue color
[11,12,15,24,25]. Copper added in similar amounts (0.2– 0.5%) to
cobalt was reported to impart blue colour to some of the Indian
glazes [26,27].
The presence of copper in both samples could be either due to its
deliberate addition as part of the manufacturing process or as traces
of raw material [12,15]. In fact, Furnival (1904) mentioned the pro-
duction of blue colour from local sand (Ajmer sand) which contains
copper and magnetic iron. The measured iron content (1.9–2.3%) is
much higher than for all the other analyzed glaze samples except
the white, which supports the mentioned historical report [3]. The
Co/Cu ratio (1:1) is the same for both samples (Table 1) [28,29]. It
is worth mentioning that the dark blue glaze contains three times
as much colouring matrix (Co and Cu) as the light blue glaze.

Fig. 3. Raman Spectra obtained from the yellow glaze layer, with first yellow particle and than orange particle, also from lead-tine yellow, type I and II (made in 1967 at the
Doerner Institut in Münchin). Laser used He/Ne at 632.8 nm.
178 S. Gulzar et al. / Journal of Cultural Heritage 14 (2013) 174–179
5.3. Green glaze
The optical microscopy and SEM examination of green glaze
sample S45G (Fig. 2d) showed a 150 to 200 ␮m thick glaze layer
with large angular quartz crystals and few irregularly distributed
small particles. Optical microscopy revealed two types of particles:
the yellowish ones are the same as in yellow glaze; the other red-
dish brown are fewer, sporadically distributed and similar to those
found in blue glazes.
The presence of lead, tin and zinc in the same ratio as for the
S32Y and S82Y yellow glazes (Table 1) suggests that green glazes
were made in part from yellow glazes [27]. Regarding the blue
colouring agents, the Cu/Co ratio of the green glaze sample dif-
fered from the ratios in the S52B and S76B blue glazes. This could
be due to an extra addition of copper into the mixture of yellow
and blue (the same previously used for the blue samples) glazes.
However, it is possible that the green glaze was obtained from a
mixture of:
• lead and tin-containing raw materials (mixed in the same pro-
portion as for the yellow glaze);
• cobalt and copper as blue colouring agents.
5.4. Purple glaze
The purple glaze sample S44P (Fig. 2e) showed a homogeneous
glaze layer of about 200 ␮m thickness with very few reddish pink
crystals under the optical microscope. The EPMA measurements
indicated that manganese (1.2%: Table 1) was used to colour the
purple alkaline glazes. This is consistent with the historic use of
manganese for purplish hues in glazes [3,12,27,30]. In addition, few
crystals of iron oxide were also observed in the glaze matrix. They
may be impurities from the raw materials.
5.5. White glaze
The examined white glaze sample S44W showed a homo-
geneous glaze layer (100–150 ␮m thick) without any type of
crystals identifiable under the microscope (Fig. 2f). The underneath
stonepaste body was whitish in tone. Therefore transparent glaze
was applied to get enriched white tonality. The composition of
the transparent glaze (Table 1) is that of typical alkaline glazes
[11,13,31].
6. Discussions
The studied glazes of uniform thickness were found to be alkali
type applied on the white stonepaste body or quartz frit [20,24].
The obtained glaze composition can be compared with other soda-
rich Islamic glazes reported from Iran and Syria but in contrast
with the high lime content (5–10%) as determined by Mason et al.
(2001). However, the lime content of the studied glazes was up
to 3.5%. This indicates the use of a particular plant ash, different
from those used elsewhere in the Islamic world [32]. The detailed
manufacturing technology of these Mughal glazes is still under
investigation to envisage the factors for the reduced lime con-
tent with unaffected magnesia levels. In contrast, similar kind of
soda-rich plant ashes with relatively same lime and magnesia con-
tent were reported from Iran, Afghanistan and Pakistan [32]. These
reports suggested the use of particular plant ashes composed of
high silica and low lime and magnesia contents which differ from
the traditionally used natron or “reh” based typical Indian glazes
in the subcontinent. The historical evidence further supports the
import of the ceramic glazed tile technology from Timurid Cen-
tral Asia during the Mughal period [7,20,31]. Rehmani (1976) also
reported the establishment of the Lahore School of Tile Decora-
tion in the reign of Mughal Emperor Shahjahan based on Timurid
traditions.
Trapped bubbles in the glazes suggest the application of glaze
suspensions on the unfired bodies as deduced from the ancient
texts [11,15]. The bubbles may result from the decomposition of
calcium carbonate during heating and fusing, after the application
of glaze suspensions on the unfired ceramic body.
The temperature calculator developed by Fluegel (2007) for
soda-lime-silica glasses [33] was used to calculate the rough
approximate temperature used for the manufacturing of Mughal
glazes. The obtained melting temperature range of 850 to 950 ◦ C is
based on silica, soda, alumina, lime, magnesia and potash values
without including the colourants amounts. The calculated tem-
perature range for glazes matches the range given in historical
reports [18–20] and has probably been used for the manufac-
turing of Mughal glazed tiles. The Raman spectra for Mughal
tile yellow glazes for the lead-tin yellow type II can also be
attributed to the same range of firing temperature (850–950 ◦ C).
The other conclusion which can be drawn (for all the glaze sam-
ples) from the above mentioned results is that the glazes were
applied to unfired ceramic body. This is because the decom-
position of calcite takes place during the same temperature
range [34]. The presence of trapped bubbles within the glaze
layer is further indicative of this calculated temperature range
(with the Fluegel temperature calculator) for firing the Mughal
glazes.
Blue, purple and white coloured glazes are thicker
(150–200 ␮m) and have higher silica content (10–12%) than
the yellow and green coloured glazes (100–150 ␮m). The yellow
and green glazes contain rapidly suspended particles of lead-tin
yellow in association with zinc. Zinc can be attributed to impurities
among the lead-tin yellow particles. The reddish toned particles
in the blue glazes are iron oxide (as determined by SEM-EDS
and ␮-XRF and also indicated by Furnival 1904), probably from
Ajmer sand, locally used to establish the blue coloured glazes
in addition to cobalt. Green glazes were manufactured with the
yellow and blue glazes or by the same raw materials. Manganese
was used to make the purple-coloured glazes in which iron oxide
was found as an associated impurity. Mughals particularly have
used transparent glaze over the whitish stonepaste body to get the
white coloured glaze tiles.
7. Conclusions
For the first time, multi-analytical techniques (OM, SEM-EDS,
RS, and EPMA) were employed to identify the colouring in the 17th
century Mughal glazes. They are characterize as plant ash alkali
glazes with low lime content as glazes reported from Timurid Cen-
tral Asia. This similarity confirms the historical route that followed
the tiles manufacturing technology from Central Asia. The glassy
glazes were manufactured at high temperatures (850–950 ◦ C) and
afterwards fused with metallic oxides obtained from the reduction
of raw materials.
The lead-tin yellow type II imparted yellow glazes; cobalt-
copper based raw materials yielded blue colours, manganese was
used for purple and a transparent glaze for white glazes. The green
coloured glazes were obtained either by mixing lead-tin yellow and
cobalt-copper blue glazes or with the addition of oxides (Pb, Sn, Cu
and Co) directly to the glassy glaze content.
Appropriate materials and conservation methods in accordance
with the glaze compositions characterized here and following the
same, high temperature manufacturing technology used in the
Mughal period can now be carefully selected to restore this dec-
orative art in Pakistan.
 S. Gulzar et al. / Journal of Cultural Heritage 14 (2013) 174–179
Acknowledgements
The authors would like to thank the College of Earth and
Environmental Sciences of the University of the Punjab-Lahore
(Pakistan), the Department of Earth Sciences of the Swiss Federal
Institute of Technology, ETH-Zurich (Switzerland) and the con-
servation research laboratory of the Collections Center from the
Swiss National Museum (Switzerland) for their collaboration in
conducting this research. We would also like to acknowledge the
anonymous reviewers for their comments that further helped in
the refinement of the research paper.
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