Journal of Archaeological Science: Reports 19 (2018) 148–154

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FTIR analysis and 3D restoration of Transylvanian popular pottery from the T

XVI-XVIII centuries
⁎
C. Măruţoiua, I. Bratub, M.I. Ţiplicc, V.C. Măruţoiua, O.F. Nemeşa, C. Neamţud, A. Hernanze,
a
Babeş-Bolyai University, Faculty de Orthodox Theology, Episcop Nicolae Ivan st., 400692 Cluj-Napoca, Romania
b
National Institute for Research and Development of Isotopic and Molecular Technologies, 67-103 Donat st., 400293 Cluj-Napoca, Romania
c
Lucian Blaga University Sibiu, Faculty of Social and Human Sciences, 5-7 Victoriei Blvd, 550023 Sibiu, Romania
d
Technical University of Cluj-Napoca, 400114 Cluj-Napoca, Romania
e
Departamento de Ciencias y Técnicas Fisicoquímicas, Facultad de Ciencias, UNED, Paseo de la Senda del Rey 9, E-28040 Madrid, Spain

A R T I C L E I N F O A B S T R A C T

Keywords: The Fourier transform infrared spectra of Transylvanian pottery fragments from XVI-XVIII centuries and the
FTIR spectroscopy of ceramics identification of their vibrational frequencies and curve fitting of the 1400–800 cm−1 spectral massif have al-
Transylvanian pottery lowed to determine the chemical and mineralogical composition of the fragments and their firing temperature. A
Ceramics firing temperature pottery vessel was restored in a virtual environment by using 3D laser scanning and computer aided design
3D pottery restoration
software. An additive manufacturing solution was used for 3D printing of the inner pottery support to reassemble
the fragments in order to assist classical restoration activities. The digital restoration allows for correct spatial
positioning of the ceramic vessel fragments and 3D modelling of the vessel shape using the profile obtained after
matching the fragments.

1. Introduction
The popular Romanian pottery originates from the old Cucuteni
Culture pottery. Between 1885 and 1910 archaeological investigations
in the Cucuteni locality (Moldova region, Romania) revealed ceramic
pots dating from 4000 to 3000 - BC. Keeping with tradition, popular
craftsmen from XVI-XVIII centuries were manufacturing ceramics by
starting with the clay that was portioned, water treated and then left to
settle from a few days to several months. After that the clay was cut in
pieces (Slătineanu, 1938, 1958; Godea, 1995). These pieces were bat-
tered with wooden hammers, wetted and laid on cow skin and further
battered with hands or feet for a few hours. This allowed for the re-
moval of stones and other hard objects from the clay. When the clay
pieces became soft and elastic they were placed on a wheel and the
shaping process started. After the pots were shaped, they were wiped
with a wet piece of leather and then left to dry for a few days in the
shadow. Next the pots were wetted and covered with varnish (a mixture
of clay and water with a specific colour). They were dried again and
then fired in kilns built from bricks and woven twigs. The temperature
was carefully controlled (850-900 °C) especially during the first firing,
which was made using wood, and endured between five and 10 h. Then
the pots were left to cool down slowly for roughly 12 h. The glazing
consisted in coating the fired pottery with a layer of clay and natural
pigments followed by a new firing that took 7 h. The red was obtained
from an iron oxide rich earth, the white from limestone and the green
from burning copper in the kiln, grinding the obtained dross and mixing
it with clay.
There are two types of ceramics based on the firing process: oxi-
dation (red ceramics) or reduction (black ceramics). Black ceramics
from Dacian origin can be found in Moldova region and northern
Transylvania. Red ceramics has a Roman origin and can be glazed or
unglazed. Unglazed pottery comes from the Roman tradition and the
glazed one with a vivid colouring follows the Byzantine style (Nicolescu
and Petrescu, 1974; Dolea, 1987; Florescu, 1958). From an artistic
point of view the first signs of independent ceramic creation emerge
towards the end of the XIV century and the beginning of the XV century.
The popular Romanian pottery is developed during the XVI-XVIII cen-
turies (Svinţiu, 2008). The studied objects come from an archaeological
dig site in the Railway Station Square of Sibiu, Romania. Different
fragments of cooking pots, jugs for water and wine keeping and
transportation were discovered in this site. It seems that an inn existed
in the area based on the large quantities of popular pottery found there.
The aim of this paper was to investigate the mineralogical composition
and firing temperatures of pottery fragments from a bowl of this site by
Fourier transform infrared spectroscopy, FTIR. Their colour, decora-
tion, thickness, shape and spectroscopic analyses are used to establish

⁎
Corresponding author.
E-mail address: ahernanz@ccia.uned.es (A. Hernanz).

https://doi.org/10.1016/j.jasrep.2018.02.044
Received 31 October 2017; Received in revised form 14 February 2018; Accepted 27 February 2018
2352-409X/ © 2018 Published by Elsevier Ltd.
C. Măruţoiu et al. Journal of Archaeological Science: Reports 19 (2018) 148–154

Fig. 1. Photographs of the pottery fragments studied by FTIR spectroscopy. Their labels, 1–4, correspond to the sample numbering. The 3a and 3b photographs are different views of the
same fragment.

Fig. 2. 3D printing of the reconstructed model of the bowl.

relationships among them and to attempt to restore an original pottery
vessel. Scanning, 3D modelling, reconstructions and visualizations are
very useful in different archaeological contexts, from representations of
complex sites and architectural reconstructions (Pejic et al., 2017;
Garstki et al., 2015) to individual objects (Marutoiu et al., 2017; Bratu
et al., 2017; Onmek et al., 2017; Carrozzino et al., 2014). Digital re-
construction of ceramic vessels is a topic addressed by many
researchers, in an effort for developing an automated system for ar-
chaeological classification and reconstruction of ceramics (Kampel and
Sablatnig, 2003), using different techniques like surface marking in-
formation with anchor points on the fragment borders (Cohen et al.,
2013) or colour markings and anchor points on surface breaks (Cohen
et al., 2016). Physicochemical analyses provide additional and very
useful information for reconstruction tasks (Rahim, 2016). Therefore, a

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Fig. 3. FTIR spectra of the pottery fragments 1 (red) and 2 (blue) in the 4000–400 cm−1
spectral region. The stretching, ν(OH), and bending, δ(HOH), vibrational bands are in-
dicated. (For interpretation of the references to colour in this figure legend, the reader is
referred to the web version of this article.)
Fig. 5. FTIR spectra from different areas of the bowl fragment 3 in the 2000–400 cm−1
spectral region. Brown area of the bowl handle (Figs. 1–3a): spectrum 3 (black line).
White-green, green and brown areas of the internal face of the fragment (Figs. 1–3b):
spectra 3 white-green (green line), 3 geen (blue line) and 3 brown (brown line) respec-
tively. (For interpretation of the references to colour in this figure legend, the reader is
referred to the web version of this article.)

Table 1
Assignment of the absorption infrared bands.

Wavenumber/cm−1 Assignment

Primary phase Secondary phase

3450 vb ν(OH), water

1640 b δ(HOH), water
1430 w ν3(CO32−), carbonates
1382 vvw ν3(NO3−), nitrates
1160 s-m Anorthite
1122 m-w Orthoclase
1043 vs-s Orthoclase
1080 s-w Quartz
996 s-vvw Muskovite
950 s-m Anorthite
920 vvw Diopside/wollastonite
862 vvw Diopside/wollastonite
877 vvw Calcite
Fig. 4. FTIR spectra from grey internal face (blue line) and the external face (black line)
795 w Quartz
areas of the bowl fragment 2 in the 2000–400 cm−1 spectral region. (For interpretation of
775 w Quartz
the references to colour in this figure legend, the reader is referred to the web version of
725 vvw M-O, ceramics
this article.)
695 vvw Quartz
648 vvw M-O, ceramics
580 vvw Magnetite
3D scanning procedure was applied to these fragments in order to re-
540 vvw Haematite
construct a bowl to a shape near to the original one. Thus, chemical and 465 m Microcline
physical contributions to the study of Transilvanian pottery from the
XVI-XVIII centuries are proposed. Types of vibration: ν, stretch; δ, bend. Labels: vb, very broad; b, broad; vs, very strong; s,
strong; m, medium; w, weak; vw, very weak; vvw, very very weak; M-O, metal‑oxygen
vibration.
2. Experimental
was done using Creaform GO!Scan 50, the preliminary results were
Four pottery fragments (shards) of one bowl obtained from the in-
processed with VXElements and the final reconstruction was done in
dicated site have been studied by FTIR spectroscopy (Fig. 1). They were
Catia V5. The 3D printing of the reconstructed vessel was done using
cleaned by mechanical methods and washed with water after the ex-
Cube Pro Duo 3D printer (Fig. 2).
traction to avoid chemical contamination. Several mg of sample
(1–3 mg) were removed from each pottery fragment. They were ground
into an agate grinding mortar, mixed with 300 mg of desiccated KBr 3. Results and discussion
Merck (spectroscopic purity degree Uvasol®) and pressed into KBr
pellets. The FTIR spectra were recorded with a JASCO FTIR 6100 3.1. FTIR spectra of the pottery fragments and mineral composition
spectrometer in the 4000–400 cm−1 spectral domain with a resolution
of 4 cm−1 using the well-known KBr pellet technique. FTIR spectra of pottery fragments in different spectral ranges are
Curve fitting with Gaussian functions of spectral regions was carried shown in Figs. 3–5.
out with the Origin 8.0 software. Digitisation for the ceramic fragments The analyses of the FTIR spectra indicate the presence of several

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Fig. 6. Minerals identified by curve fitting to the 800–1400 cm−1 spectral massif in the bowl fragments. 1, fragment 1; 2, fragment 2, external face; 3, fragment 2, grey internal face; 4,
fragment 3, brown area of the handle; 5, internal face of the fragment 3, white green area; 6, idem, green area; 7, idem, brown area; 8, fragment 4. Labels: A, anorthite (red); M, muscovite
(green); O, orthoclase (blue); Q, quartz (magenta); C, calcite (dark yellow). (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of
this article.)

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Fig. 7. FTIR spectra of the bowl fragments 1 (red), 2 internal face (blue) and 4 (green).
The vertical line indicates the wavenumber of the maximum of the SieO stretching region
corresponding to clay used in pottery at 100 °C (Damjanovic et al., 2014). (For inter-
pretation of the references to colour in this figure legend, the reader is referred to the web
version of this article.)

components in the pottery samples, Table 1. The bands observed at

3450 and 1640 cm−1 are assigned respectively to the OeH stretching
and HeOeH bending vibrations of the water molecules included in the
bowl minerals. The bands at 795, 775 and 695 cm−1 reveal the pre-
sence of quartz, whereas the bands at ~580 and ~540 cm−1 are signals
of the content of the iron oxides magnetite and haematite respectively
(Dhanapandian et al., 2012).
The band at ~1430 cm−1 in the spectra of the grey area of the
fragment 2, Fig. 4, is assigned to the ν3 degenerate stretching, E', mode
of the CO32– group, indicating the presence of carbonate residues
(Ayora-Cañada et al., 2012). Nitrate, NO3−, residues are also detected Fig. 9. Reconstructed digital 360° view of the bowl from its fragment 1.
in this fragment (peak at ~1382 cm−1) and in the fragment 3, Fig. 5.
The presence of nitrates in the buried bowl could be due to con-
tamination with decomposed organic matter from the site (Hernanz 2008), assigned to different vibrations of SieO type (Shoval et al.,
et al., 2006). The wavenumber of the observed peak (assigned also to 2011). The crystalline phase content increases with firing temperature.
the ν3 degenerate stretching, E', mode of the nitrate group) suggests the The broad band at ~1030 cm−1 indicates the destruction of octahedral
presence hydrated NO3− clusters (Pathak, 2012), something expected sheet structure around ~650 °C, and the presence of the bands at 535
in decomposed organic matter and not in a fired object. The intense and 585 cm−1 confirms the complete re-oxidation of iron compounds
absorption band at ~465 cm−1 is assigned to the feldspar microcline (Ravisankar et al., 2010; Baritone et al., 2011).
(Palanivel and Kumar, 2011). The bands at ~725 cm−1 and 648 cm−1 Feldspars (orthoclase, microcline and anorthite), quartz and calcite
are attributed to metal‑oxygen vibration from ceramics (Shoval et al., are usual minerals found in pottery (Legodi and de Waal, 2007; Ayora-
2011). The crystalline phases of diopside and gehlenite type are re- Cañada et al., 2012). Several infrared bands of these minerals overlap
presented by the vibrational frequencies beneath the spectral massif giving rise to the strong spectral massif observed in the 800–1400 cm−1
between 1300 and 850 cm−1 (De Benedetto et al., 2005; Barilaro et al., range of the spectra of the bowl fragments, Figs. 3–5. Curve fitting to

Fig. 8. Digital image of the fragment 1 of the bowl indicating production traces, reference plane and its symmetry axis.

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Fig. 10. 3D printed model of the bowl supporting different ceramic fragments.
this massif with Gaussian components, recognised previously by second
derivative treatments (Akyuz et al., 2008), has made possible the
identification of minerals present in the bowl, Fig. 6.
The feldspars anorthite (bands at 1160 and 950 cm−1) and ortho-
clase (bands at 1122 and 1043 cm−1) are some of the minerals of the
bowl that contribute to the studied spectral massif. Other identified
components are quartz (band at 1080 cm−1), muskovite (band at
996 cm−1) and calcite (band at 877 cm−1), (Cugalj et al., 2008). Ac-
cording to these results, fragments 1, 2 and 3 have a similar miner-
alogical composition and different from that observed in the fragment
4. The latter does not contains calcite but the spectral profile suggests
the presence of diopside/wollastonite (characteristic absorption bands
located at ~920 and 862 cm−1 (Barilaro et al., 2008). Heterogeneity in
the distribution of the materials in the bowl could explain these dif-
ferences in the composition of its fragments.
3.2. Firing temperature
The two common ways for the firing process in pottery are the use of
an open fire or a kiln. The open fires reach a maximum temperature of
about 800 °C (Bollang et al., 1993), whereas the kilns used for this
purpose may reach 1230 °C. Infrared spectroscopy is a useful technique
to determine the firing temperature of pottery (Legodi and de Waal,
2007; Ayora-Cañada et al., 2012; Damjanovic et al., 2014). The calcite
impurity in ancient ceramics is used as a marker for the reconstruction
of the firing conditions (Wopenka et al., 2002). The identification of
traces of calcite would suggests a firing temperature of about 800 °C
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Journal of Archaeological Science: Reports 19 (2018) 148–154
(Ayora-Cañada et al., 2012), although a post-burial re-carbonation
process cannot be excluded. The orthoclase content in clays diminishes
when firing from 800 °C to 1100 °C and completely disappears at
1200 °C (Johari et al., 2010). The infrared spectral massif between 1300
and 850 cm−1 is dominated by the SieO stretching bands of the sili-
cates contained in the pottery. The maximum of this strong and broad
feature of the spectra is influenced by the firing temperature used in
pottery manufacture (Damjanovic et al., 2014). The absorbance max-
imum of the SieO stretching region shifts towards higher frequencies
and broadens with increasing temperature. The maxima and spectral
profile observed in the bowl, Fig. 7, indicate that the firing temperature
can be estimated at ~800 °C (Damjanovic et al., 2014). Therefore, the
bowl was fired at relatively low temperature, not exceeding 800 °C,
which suggests the use of open fire.
3.3. 3D reconstruction
The ceramic fragments of the studied bowl come from its bottom;
the top of the bowl is missing. Because of this it cannot be completely
restored in a digital format. The digital restoration has two objectives:
to identify the correct spatial position of each fragment generating the
profile of the most complete bowl section, and the second objective is to
build a 3D model by printing an inner support (identical to the bowl
shape) to place the ceramic fragments on.
The digital reconstruction of the bowl was done using an algorithm
similar to those developed previously (Calin et al., 2011; Neamtu et al.,
2012). The first stage was the digitization of the ceramic fragments. The
C. Măruţoiu et al.
seven pieces were scanned with GO!Scan 50. The second stage was
determining the symmetry axis of each fragment. For this task each
fragment is visually inspected identifying the orientation of the pro-
duction traces. From this information a plane is defined parallel with
these traces (horizontal reference plane). The digitized fragment is in-
tersected with this plane and with another plane parallel to the hor-
izontal reference plane in order to obtain a series of concentric circles,
Fig. 8. The center of this circle is used to determine the symmetry axis.
The symmetry axis and the horizontal reference plane are used to ob-
tain the profile of the ceramic fragment using the intersection between
a plane and the surface of the ceramic fragment. The resulted profile is
rotated around its symmetry axis to obtain a 360° view of the bowl,
Fig. 9. For each digitized fragment, the process described above is re-
peated.
Using additive manufacturing the reconstructed model of the bowl
was printed and used as support for different ceramic fragments as
presented in Fig. 10.
4. Conclusions
The chemical and mineralogical composition of the ceramic shards
has been proposed from a FTIR analysis (curve fitting of the
1400–800 cm−1 spectral massif). The firing temperature has also been
estimated at about 800 °C from their FTIR spectra. The pottery was
restored in virtual environment using 3D laser scannig and the adequate
software. Computational 3D reconstruction together with physical and
chemical analyses is very useful to restore the original bowl. The 3D
printing of the bowl cavity provides a printed support very useful to
reassemble the shards in order to proceed for its classical restoration.
Therefore, significant chemical and physical contributions to the study
of Transilvanian pottery from the XVI-XVIII centuries have been
achieved.
Disclosure
C. Măruţoiu and I. Bratu are co-first authors.
Acknowledgments
Thanks are due to UEFISCDI for financial support of the PN II-PT-
PCCA-2013-4-1882 project. Two referees and the co-editor Chris O.
Hunt offered comments that improved the manuscript.
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