A. S. MATHEW et al.: CHARACTERISATION AND OSL DATING OF AN ANCIENT BRICK ...
791–797
CHARACTERISATION AND OSL DATING OF AN ANCIENT
BRICK WELL AT PATTARAIPERUMBUDUR, TAMIL NADU,
INDIA
KARAKTERIZACIJA IN DATIRANJE STARODAVNEGA
OPE^NATEGA VODNJAKA V PATTARAIPERUMBUDURU, TAMIL
NADU, INDIJA
Alby Sara Mathew
1
, Minnoo Grasa Abraham
1
, Thirumalini Selvaraj
1*
,
Baskar Jaganathan
2
1
School of Civil Engineering, Vellore Institute of Technology, Katpadi Road, VIT campus, Vellore, Tamil Nadu 632014, India
2
Department of Archaeology, Tamil Nadu 602023, India
Prejem rokopisa – received: 2020-06-22; sprejem za objavo – accepted for publication: 2020-07-15
doi:10.17222/mit.2020.042
This paper is about characterizing a brick sample obtained from the brick well at Pattaraiperumbudur, a recently excavated site
in Tiruvallur, Tamil Nadu. The petro-archaeometry studies of this site included the findings about its elemental constitution,
mineralogical composition, thermal changes and physical properties. The elemental constitution was determined using an XRF
test, while the mineral composition was found with the help of XRD and FT-IR, showing the chemical bonding at various peaks.
A material can undergo different thermal reactions at various temperatures and the effect of temperature on the sample was
screened through a TG-DTA analysis. Optical microscopy (OM) is one of the important tests used in petro-archaeological stud-
ies, confirming the XRD results. The morphology of the sample was studied with the aid of FE-SEM, which provided an idea
about the porous structure and elemental composition. Physical tests of water absorption, porosity and bulk density provided in-
formation on the durability of the brick sample. The combined results of TGA and XRD suggest that the firing of the bricks had
taken place below 950 °C in an oxidising atmosphere. The chemical composition reveals that the clay contains a low amount of
CaO and the flux concentration is greater than 9 %, indicating low refractory. The extracted brick samples were subjected to car-
bon dating using optically stimulated luminescence (OSL) that found them to be 2100 years old. 3D rendering of the well was
created with the help of the H-BIM tool.
Keywords: mineral characterisation, microstructural analysis, OSL dating
V ~lanku avtorji opisujejo karakterizacijo vzorca opeke, vzetega iz ope~natega vodnjaka v Pattaraiperumbuduru, kjer so
nedavno izvedli geolo{ka izkopavanja v Tiruvallurju, Tamil Nadu, v Indiji. Petro-arheolo{ke {tudije tega nahajali{~a obsegajo
raziskovanje osnovne kemijske zgradbe, mineralo{ke sestave, termalnih sprememb in fizikalnih lastnosti izkopanih vzorcev.
Kemijsko sestavo vzorcev so dolo~ili z rentgensko fluorescenco (XRF), medtem ko so mineralo{ko sestavo dolo~ili z rentgensko
difrakcijo (XRD) in Fourierjevo transformacijsko infrarde~o spektroskopijo (FT-IR). Material med segrevanjem in ohlajanjem
lahko do`ivi vrsto sprememb. Te so opazovali s pomo~jo termo-gravimetrije (TG) in diferencialne termi~ne analize (DTA). S
pomo~jo opti~ne mikroskopije (OM), ki je ena od osnovnih metod petro-arheolo{kih raziskav, so potrdili rezultate dobljene z
XRD. Morfologijo vzorcev so {tudirali z vrsti~no elektronsko mikroskopijo na poljsko emisijo (FE-SEM), ki lahko pomaga pri
opisu porozne strukture in kemijske sestave. Fizikalne preiskave, kot so na primer dolo~itev absorpcije vode, poroznosti in
volumske gostote, podajajo informacijo o dobi trajanja oz. starosti vzorcev opeke. S kombiniranjem rezultatov TGA in XRD so
avtorji ugotovili, da je bila opeka `gana pod 950 °C v oksidacijski atmosferi. Kemijska analiza je pokazala, da glina vsebuje
majhno vsebnost CaO in da je vsebnost talil ve~ja kot 9 %, kar ka`e na to, da ima analizirana opeka slabo ognjevzdr`nost.
Izkopani vzorci opeke so bili datirani z ogljikom oz. uporabo opti~no simulirane luminescence (OSL). Datiranje je pokazalo, da
so vzorci stari 2100 let. 3-D prikaz vodnjaka so obnovili in predstavili s pomo~jo programskega orodja H-BIM (angl.; Heritage
Building Information Modeling).
Klju~ne besede: mineralo{ka karakterizacija, mikrostrukturna analiza, datiranje z opti~no simulirano luminescenco (OSL).
1 INTRODUCTION
This paper highlights important correlations between
civil-engineering, archaeological and architectural val-
ues. The civil-engineering aspect involves the study of
the materials and production technology adopted during
a construction; the archaeological aspect involves the in-
vestigation of the period, in which the structure was
built; the architectural aspect tells us about the creative
ideas of ancient people. When we look into our past, we
find many vital structures and monuments, which had
been constructed in the early centuries. The technology
used then is still a mystery to the present generation. So,
it is of utmost importance to determine the methods and
techniques used in our country for the construction of
these ancient heritage structures. This study includes a
characterisation of the building materials. The charac-
terisation process includes mineralogical, elemental and
textural detailing of the sample.
1
This kind of study is
termed as petro-archaeometry.
Bricks are one of the most ancient building materials
known to us. The aesthetic aspect of brick work has
Materiali in tehnologije / Materials and technology 54 (2020) 6, 791–797 791
UDK 620.1:67.017:549.514.6 ISSN 1580-2949
Original scientific article/Izvirni znanstveni ~lanek MTAEC9, 54(6)791(2020)
*Corresponding author's e-mail:
thirumalini.selvaraj@vit.ac.in (Thirumalini Selvaraj)

gained a lot of consideration over the years. The historic
relevance of these ancient structures or monuments is of
utmost importance not only for the analyses and preser-
vation process but also for understanding the technolo-
gies used by the ancient people; besides, these structures
connect the ancient and modern era. The knowledge of
the raw materials used in construction process is very
important for the restoration of ancient structures.
2
The study of ancient structures has always been cru-
cial in our research area.
4
The wide research in this area
helps us understand the evolution of construction tech-
nologies and the living style of our ancestors.
4
The po-
tentials of the study of heritage science are enhanced
with the help of petro-archaeometric studies, analysing
the chemical compositions of the materials used for the
construction of these structures.
3,4
Pattaraiperumbudur is an archaeologically important
site excavated in the village of Tiruvallur, Tamil Nadu.
Numerous archaeological artefacts from the prehistoric
period to the early historic period were found during the
excavation. These include pottery, stone tools and bricks,
which represent the Palaeolithic culture of the site. Apart
from the stone-age tools, the remnants of the iron-age
culture were also identified. During the excavation, a
brick well was found at a depth of 2.85 m. Based on a vi-
sual inspection, a sample brick seemed less porous and
comparatively larger than the present bricks, rectangular
and orange-red in appearance. No salt efflorescence that
reduces a major stress caused to bricks was observed.
2
In order to find the technologies used in the manufac-
turing of building materials, the characterisation of the
brick sample was important.
5
The characterisation in-
cluded the study of the physical properties, mineral com-
position, thermal reactions during the baking process and
also the microstructure of the material.
2,3
The physical
properties studied were the water absorption, porosity
and bulk density.
10
The water absorption is proportional
with the porosity. The chemical composition of the sam-
ple was determined with XRF. With the help of the XRF
data, the type of clay was determined with respect to
whether it was a calcareous or non-calcareous sub-
stance,
6
while a TG-DTA analysis helped us understand
the firing temperatures and weight loss due to the ther-
mal activity.
2,6
Mineralogical analyses were performed
with the help of X-ray diffraction.
2,3,4
Petrographic and
microstructural studies were carried out with the help of
optical microscopy (OM). The texture level of the vitrifi-
cation and the pore size were evaluated with the help of
FE-SEM.
1,8
EDS gave the elemental composition for a
particular region of the sample.
3,14
FT-IR helped us study
chemical reactions such as decomposition, dihydro-
xylation and deconvolutions associated with heating.
9,10,13
OSL dating gave the information about the age of the
sample.
21
Dating can be done using two methods,
thermoluminescence and optical luminescence. In this
project, optically stimulated luminescence was carried
out. Some minerals are capable of storing a small
amount of energy derived from the radioactive elements
such as uranium, thorium and potassium when they are
exposed to radioactive decay. Later, the ejected electrons
and holes recombine with the opposite charges when the
light is stimulated and thus luminescence of the sample
is formed.
23
We also used the terms equivalent dose,
which is the amount of energy absorbed by a buried sam-
ple, and dose rate, which is the measurement of the en-
ergy absorbed every year from the radiation present in
A. S. MATHEW et al.: CHARACTERISATION AND OSL DATING OF AN ANCIENT BRICK ...
792 Materiali in tehnologije / Materials and technology 54 (2020) 6, 791–797
Figure 2: Brick well and the brick sample Figure 1: Ariel view of the Pattaraiperumbudur excavated site

the surrounding environment. Dating techniques were
mainly used by the department of archaeology for deter-
mining the era of the construction of the remains ob-
tained from the excavation site. Figure 1 shows the ariel
view of the site.
2 MATERIALS AND METHOD
2.1 Collection of samples
The site of Pattaraiperumbudur contributes signifi-
cantly towards the knowledge about ancient settlements.
The site lies on the eastern bank of the Kosathalaiyar
River. A number of sites on the bank of the Kosatha-
laiyar River have a great significance for the Indian
Palaeolithic archaeology. An archaeological team carried
out an excavation between May and September 2018.
The sampling of well was done under the guidance of the
officials from the Department of Archaeology, Tamil
Nadu. A brick sample was removed from the top course.
Many trenches with sizes of 10m×10mand4.25 m ×
4.25 m were dug during the excavation at the
Pattaraiperumbudur site. The brick well was found in
trench B1 at a depth of 2.85 m. From the preliminary ex-
amination of the site, information regarding the size,
depth and nature of the soil was obtained. The depth
from the first course to last course of the well is about 3.
91 m. The exterior and interior diameters of the well are
2.60 m and 2. 20 m. The number of brick courses is 52
and each course consists of 32 bricks. The average size
of a brick is 24 cm × 24 cm×7cm.Figure 2 shows the
well and the brick.
2.2 Optical microscopy
The mineral composition was observed using a Zeiss
optical microscope. Thin polished sections required for
optical microscopy were prepared at Chennai, Tamil
Nadu. Petrographic sections were prepared by cutting a
slice of the sample with a thickness of 0.03 mm, which
was then attached to a glass slide with epoxy resin and
covered with a glass slip. This slide is examined under a
polarising microscope.
2.3 X-ray diffraction (XRD)
A Siemens D500 Advance diffractometer using Cu-K
radiation, equipped with a NaI (Tl) scintillation detector
was used for the XRD analysis. Samples of about 5–10
mg were finely ground, sieved through a 45-micron sieve
and used for the analysis. XRD provided the mineral
composition of the brick sample. The Xpert high-score
software was used to identify the mineralogical composi-
tion.
2.4 Fourier transform infrared spectroscopy (FT-IR)
An IR Affinity-1 using software IR Solution 1.60
with a resolution of 0.5–16cm
–1
was used for the FT-IR
spectroscopy. The instrument has a precision of ±5 cm
–1
.
This investigation was done using the KBr pellet tech-
nique, whose wave number ranged from 4000 cm
–1
to
400 cm
–1
and also by mixing the powdered samples with
KBr in the 1:20 weight proportion. A sample of about
5–10 mg was required for the analysis; infrared radiation
was applied to it, some of which was absorbed by the
sample while some passed through it. Each molecular el-
ement has a different infrared pattern; thus, functional
organic and inorganic groups can be identified.
2.5 Field-emission scanning electron microscopy
(FE-SEM)
A morphological study of the samples was carried
out using a Thermo Fisher FEI QUANTA 250 FEG
equipped with a Schottky field-emission electron gun as
the electron source. It provides a high resolution of 1.2
nm at 30 kV and high vacuum in an operating voltage
range of 5–30 kV. The sample used for the analysis was
sputter coated with a very thin gold layer, resisting the
charging and the sample was magnified in a range of
5–10.000 kX with a spot energy-dispersive spectrometer
(EDS) to evaluate the elemental composition of the sam-
ple.
2.6 X-ray flourescence (XRF)
The elemental bulk compositions of the finely ground
<45 μm powder as lime-paste reproductions in w/% ox-
ides were obtained using a JEOL JS83201Z X-ray fluo-
rescence spectrometer. About 10 g of powder was in-
serted into the sample tube of a 3628 Bench–Press Spex
Cretiprep disc press machine to form a thin sample plate
at a pressure of 20 tons in 2 min. The resulting sample
disc was placed into the sample holder of the X-ray fluo-
rescence spectrometer and the analysis of each oxide was
performed within an error of 0.01 w/%.
2.7 Thermogravimetric analysis (TGA)
TG-DTA analyses were carried out using a SDT
Q600. It has a heating rate of 5–20 °C/minute. Samples
can be heated in nitrogen up to 1200 °C. Dried powdered
samples of 5–10 mg were used for the analysis, during
which the rate of change in the weight of a sample as a
function of temperature or time was measured in a con-
trolled atmosphere.
2.8 Optically stimulated luminescence (OSL)
The lab was equipped with a TL-DA-15 lumines-
cence reader and alpha counter to determine the uranium
and thorium contents in a sample. The sample prepara-
tion was done under subdued-red-light conditions. Blue
or green light was used when dealing with quartz and in-
frared light was used for feldspar. The single-aliquot pro-
tocol (SAR) was followed. In the preliminary treatment,
first the sun-exposed layers were filed off and crushed in
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Materiali in tehnologije / Materials and technology 54 (2020) 6, 791–797 793

a beaker where the removal of carbonates and organics
was done with chemical solutions. Density separation
was done to separate quartz and feldspar; etching was
also done to remove the alpha skin. The preliminary
treated sample was then fixed to the stainless disc using
silicon spray. About 35 discs were prepared for each
sample and run for the test dose. The equivalent dose
was calculated using Duller’s Analyst software.
Grun’s software was used for the age estimation.
Age of the sample = equivalent dose/annual dose rate
2.9 Mechanical and physical properties
The mechanical property was determined with the
compression test performed on extracted samples, while
the physical tests determining the water absorption, po-
rosity and bulk density were carried out in accordance
with IS 3495 (Part 1-4): 1992. The compression testing
was carried out at a loading rate of 1.28 KN/sec [IS 3495
PART 1: 1992].
Water absorption (%) was calculated using formula
[M
2
– M
1
] × 100/M
1
.
Porosity (%) = [(M
2
– M
1
)/(M
2
– M
3
)] × 100
Bulk density = [M
1
/(M
3
– M
2
)] × 10³,
where
M
1
= mass of an oven-dried specimen;
M
2
= mass of a saturated specimen;
M
3
= hydrostatic mass.
Compressive strength = maximum load at failure/net
area of faces under compression.
2.10 Structural drawing
3D modelling was done to get the accurate dimen-
sions and a perfect model of the well. It was done with
the help of the H-BIM tool. The images required for the
modelling were captured with a Kinect sensor and the
Context Capture software was used for the modelling.
3 RESULTS AND DISCUSSION
3.1 Optical microscopy
The thin sections were examined with a polarising
microscope and the pictures included in Figure 3 were
A. S. MATHEW et al.: CHARACTERISATION AND OSL DATING OF AN ANCIENT BRICK ...
794 Materiali in tehnologije / Materials and technology 54 (2020) 6, 791–797
Figure 3: Optical microscopy: a, b) quartz; c) feldspar; e, f) boromuscovite
Figure 4: XRD of the brick sample

obtained. In the polarized-light microscope, the bending
of planar morphological elements such as rational crystal
or cleavage indicate plastic crystal deformation.
25
From
these images, the presence of quartz, feldspar, hematite
and boromuscovite can be identified.
25
3.2 XRD
The XRD plots were recorded in a 2 range of
10–90°. The XRD analysis of the brick sample in Fig-
ure 4 indicates the presence of quartz, boromuscovite,
berlinite, anorthite and feldspar. It also indicates the
phase transformation of calcite into anorthite at different
sintering temperatures.
10
The XRD results are consistent
with the FT-IR analysis which shows broadening peaks
at 1100–1000cm
–1
, referring to the amorphization reac-
tion.
3.3 FT-IR
Figure 5 depicts the FT-IR spectra of the brick sam-
ple. The deconvolution of the peak range between
2450–2000 cm
–1
and 1200–800 cm
–1
indicates the expo-
sure of the brick sample to different firing temperatures.
9
The broad absorption band at 1031.92 cm
–1
is of an
asymmetric Si-O stretching followed by a strong absorp-
tion band at 445.56 cm
–1
, also indicating the presence of
quartz.
9,10
The highly sensitive carbonate band, which
normally shows at around 1400 cm
–1
for a sintered sam-
ple was not found for this sample, indicating the trans-
formation of calcite to anorthite.
10
The peak at
534.28cm
–1
corresponds to the Fe-O bending of hema-
tite.
14
3.4 FE-SEM
The scanning-electron-microscope observations pro-
vided valuable information about the internal morphol-
ogy, distribution matrix, pore-structure formation and
size of the crystals.
14
This sample contains pores, which
are of a medium size, and it is less vitreous in nature, in-
dicating that the temperature, at which the sample was
fired was less than 950 °C.
23
The presence of feldspar
and the accumulation of quartz crystals that are in agree-
ment with the XRD and FT-IR results are shown in Fig-
ure 6.
3.5 XRF
Table 1 lists the XRF-analysis results confirming that
the brick sample contains high concentrations of SiO
2
,
Al
2
O
3
and very low amounts of Na
2
O, MgO and CaO.
Since the amount of calcium present is lower than 6 %,
the clay used for the manufacturing of bricks was
non-calcareous.
6,14
Since the amounts of inorganic oxides
such as Fe
2
O
3
, MgO, CaO, etc. are higher than 9 % by
weight, they indicate fluxing and a medium refractory
property.
10
The presence of Na, Ti, Ca, Mg and K has a
non-negligible effect on the hardness of the brick.
9
Table 1: XRF data
Oxides Mass %
SiO2
66.9
Al2
O
3
17.2
Fe2O3 4.3
CaO 3.58
K2
O 3.13
Na2
O 2.12
MgO 1.27
TiO2
0.748
P2
O
5
0.297
A. S. MATHEW et al.: CHARACTERISATION AND OSL DATING OF AN ANCIENT BRICK ...
Materiali in tehnologije / Materials and technology 54 (2020) 6, 791–797 795
Figure 6: FE-SEM images: a) quartz accumulation; b) feldspar; c) porous structure
Figure 5: FT-IR peaks of the brick

3.6 TGA
The TGA curve shown in Figure 7 indicates a negli-
gible weight loss in the region of 600–900 °C, which in-
dicates the dihydroxylation of the raw materials for the
brick at the firing temperature, containing a low amount
of calcite according to the XRD analysis.
6
The weight
loss of around 1.5 % occurs in the temperature range of
200–400°C due to the loss of interlayer water and clay
dihydroxylation.
2,13
The total weight loss is less than 2 %
by weight. The firing temperature of the sample is
mostly between 750–900 °C. The absence of mullite and
cristobalite indicates that the firing temperature is below
950 °C.
6,24
The presence of anorthite indicates the de-
composition of calcite at higher firing temperatures.
2
Be-
tween 700 and 800 °C, the clay is of an orange-red
color.
14
DTA (Figure 8) shows the physical changes that
do not involve weight changes such as crystallisation,
melting, the change in the solid phase and homogeneous
reaction in the solid state.
3.7 OSL
OSL is a widely used technique in archaeological
dating.
21
The single-aliquot-regeneration (SAR) protocol
of Wintle and Murray is used for the determination of the
equivalent dose/palaeodose. The amount of the light
emitted during the luminescence measurement of the
sample depends upon the total radiation dose, to which
the crystalline material was exposed while it was buried
and it is called the natural signal. This measured signal
provides the measure of the palaeodose. The total radia-
tion dose, which a material receives annually is called
the annual radiation dose. Based on the OSL dating, the
approximate age of the sample is determined to be 2100
years. This test confirms that the well was constructed in
the Early historic period.
3.8 3D model
The modelling of the brick well was based on the
principle of photogrammetry, which is a part of
H-BIM.
22
This is a technology used for obtaining infor-
mation about objects through a process of measuring re-
corded images. The final output is obtained after going
through various stages such as the collection of images,
archaeological relevance or survey data. The images
were captured at an angle of 30° and stitched together
with an overlap of 30°. The rendered 3D model of the
brick well is shown in Figure 9.
3.9 Physical and mechanical properties
The water absorption and porosity are the key factors
in determining the durability of a brick sample. The wa-
ter absorption is relatively proportional to the porosity.
The value obtained for our sample is 15 %; therefore, the
sample is durable. The standard water-absorption value
must be less than 21 % for high-quality bricks.
9
The
value of porosity obtained is 22.8 % and the bulk density
is 1.873 kg/m
3
. The compressive strength of the brick ob-
tained is 6.7 MPa. A compressive strength between 2.5
MPa and 7 MPa is recommended for horizontally perfo-
rated bricks used for indoor constructions.
10
The values
are compared with respect to the IS Codes.
A. S. MATHEW et al.: CHARACTERISATION AND OSL DATING OF AN ANCIENT BRICK ...
796 Materiali in tehnologije / Materials and technology 54 (2020) 6, 791–797
Figure 8: DTA curve of the brick sample
Figure 7: TGA curve of the brick sample Figure 9: 3D rendering of the Pattaraiperumbudur brick well

4 CONCLUSION
From the tests conducted, it is concluded that the
bricks used in the construction of the well exhibit an op-
timum water absorption, compressive strength and
slightly porous structure. The combined results of XRD,
OM, SEM, TGA confirm the presence of minerals such
as quartz, feldspar, anorthite and boromuscovite. They
also provide an idea of the production technology used,
indicating that the bricks are non-vitreous in nature and
produced from Ca-poor clay with high amounts of silica
and alumina at a firing temperature of less than 950 °C.
The clay used in the production of exhibits inorganic
fluxing and a medium refractory property. The suitable
proportion of quartz in the clay prevents shrinkage and
warping and improves the durability of bricks.
9
The OSL
dating technique gives the age of the sample, confirming
that the brick well was constructed in the Iron Age pe-
riod.
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