E. PRIETO-VICIOSO et al.: CHARACTERIZATION OF LIME MORTAR AND PLASTERS OF FORTRESS CONCEPCION ...
533–539
CHARACTERIZATION OF LIME MORTAR AND PLASTERS OF
FORTRESS CONCEPCION DE LA VEGA
KARAKTERIZACIJA APNENE MALTE IN OMETOV TRDNJAVE
CONCEPCION DE LA VEGA
Esteban Prieto-Vicioso
1*
, Virginia Flores-Sasso
2
, Sagrario Martínez-Ramírez
3
,
Letzai Ruiz-Valero
2
, Gloria Pérez
4
1
Universidad Nacional Pedro Henríquez Ureña, Santo Domingo, Dominican Republic
2
Pontificia Universidad Católica Madre y Maestra, Santo Domingo, Dominican Republic
3
Instituto Estructura de la Materia, Madrid, Spain
4
Instituto de Ciencias de la Construcción Eduardo Torroja, Madrid, Spain
Prejem rokopisa – received: 2022-03-04; sprejem za objavo – accepted for publication: 2022-06-10
doi:10.17222/mit.2022.525
The arrival of Christopher Columbus in America stimulated the creation of new settlements in which the materials and construc-
tion methods coming from Spain and those existing in the area were used. The first village built was La Isabela (1494) where
the Spaniards found good limestone for ashlars and were able to make lime as well as good clay for earth walls, masonry walls,
etc. After La Isabela, the cities of La Vega (1495) and Santo Domingo (1498) were established. These villas still include ves-
tiges of these building materials that are a source of information about their composition. The study is focused on the ruins of
the fortress of Concepcion de La Vega that survived the earthquake in 1562 that destroyed the city. The aim of this research was
to characterize the mortar and plasters of the fortress of Concepcion de La Vega on the Hispaniola Island. To determine their
chemical and mineralogical composition optical microscopy (OM), Fourier-transform infrared spectroscopy (FTIR), Raman
spectroscopy and a thermogravimetric differential thermal analysis (TG-DTA) were used. The results showed that the major
component of the mortars was CaCO3 (95 %), indicating that there is lime mortar. The plaster is lime based with iron oxide.
Keywords: lime mortar, plasters, FTIR, Raman spectroscopy, TG-DTA
Prihod Kri{tofa Kolumba v Ameriko je spodbudil nastanek novih naselij, pri gradnji katerih so se uporabljali materiali in
tehnologije iz [panije ter tisti iz lokalnega okolja. Prva s tem pristopom zgrajena vas je bila La Isabela (1494), kjer so [panci
odkrili kakovosten apnenec za vogalne kamne ter za proizvodnjo apna, kot tudi glino ustrezne kakovosti za butane stene in
izdelavo ope~nih zidakov, itd. Po La Isabeli sta nastali mesti La Vega (1495) in Santo Domingo (1498). Tamkaj{nje vile {e
vedno vsebujejo sledove omenjenih histori~nih gradbenih materialov, ki so vir infromacij za preu~evanje njihove sestave.
Predstavljena {tudija je osredoto~ena na preu~evanje ru{evin utrdb iz Concepcion de La Vega, ki so leta 1562 prestale potres, ki
je uni~il mesto. Namen raziskave je bilo okarakterizirati malte in omete utrdb iz Concepcion de La Vega na otoku Hispaniola.
Kemijska in mineralo{ka sestava je bila dolo~ena s Fourier transformacijsko infrarde~o spektroskopijo (FTIR), Ramansko
spektroskopijo in termogravimetrijo sklopljeno s termi~no analizo (TG-DTA). Rezultati analiz so pokazali, da je bila glavna
komponenta malt kalcit (CaCO3), katerega dele` je zna{al 95 %, kar nakazuje na apneno malto. Omet je apnenega izvora z
vsebnostjo `elezovega oksida.
Klju~ne besede: apnena malta, omet, FTIR, Ramanska spektroskopija, TG-DTA
1 INTRODUCTION
1.1 General
It is well documented that one of the most popular
materials that make up the architectural heritage of hu-
manity is lime mortar, in a structural way joining stone
or brick, used for rammed earth walls as a covering or
decorative element.
1,2
Over the centuries, historic mortars
have proven to be durable and well compatible with his-
toric structural units; however, different factors (pollu-
tion, presence of water, temperature differences, pres-
ence of soluble salts, etc.) can accelerate their
deterioration.
3
The masonry walls of historic buildings degrade, de-
pending on the traditional building materials (stone,
brick, aerial or hydraulic mortars, etc.), due to the pas-
sage of time and site-specific environmental loads. How-
ever, the selection of repairs can be significantly influ-
enced by different professionals’ philosophical perspec-
tives that can be broadly categorized as purist, pragmatist
or cynic. The difference in their reporting will clearly de-
termine alterative starting positions for repair works,
with divergence in a project potentially occurring when
philosophical tenets are applied.
4
In this way, worldwide research on lime mortar and
plaster of historic buildings has been carried out. One of
the most interesting aspects is the possibility of deter-
mining what types of binder, aggregate or even admix-
ture were used and what their characteristics are.
5–8
RILEM TC 167-COM has made crucial headway in
characterizing historic masonry in chemical, mineralogi-
cal, physical and mechanical ways.
9
Durability is one of the most important properties
that a builder looks for in lime mortar. The durability re-
Materiali in tehnologije / Materials and technology 56 (2022) 5, 533–539 533
UDK 666.971.3:693.6:94(729.3La Isabela) ISSN 1580-2949
Original scientific article/Izvirni znanstveni ~lanek MTAEC9, 56(5)533(2022)
*Corresponding author's e-mail:
eprieto@unphu.edu.do (Esteban Prieto-Vicioso)

fers to the ability of a structure to maintain substantially
its original appearance, strength and soundness for many
years. In masonry the two prime requisites for durability
are a dimensionally stable unit and mortar that forms a
permanent and complete bond, thereby making the struc-
ture watertight.
10
Lime mortar and plaster have been investigated to
improve the knowledge of how to make them as durable
as before the cement technology was developed.
11
The
durability of lime mortars is directly related to their
physical properties and porosity, and there are numerous
studies about the physical properties of lime mortars.
Thirumalini et al. studied the influence of an addition of
an organic admixture on different properties of mortars.
12
Cultrone et al. and Ponce-Antón et al. studied the manu-
facturing technology and durability of lime mortars.
13,14
In America there have been few studies on lime mor-
tars and plasters, and most of them have been carried out
in Mexico. Carran et al. analyzed the first use of lime by
the Mayan civilization
2
; Rodríguez Pérez et al. studied
the physical/mechanical properties of the limestones
from the Yucatan churches
15
and Miriello et al. assessed
the hydraulicity of the lime plasters from Teotihuacan.
16
In Brazil, Gleize et al. characterized historical mortars
17
;
Loureiro et al. studied the historic mortars
18
and Gomes
de Oliveira et al. investigated the mortars and clay bricks
in historic structure from the 18
th
century.
19
In Peru,
Morillas et al. carried out the characterization of restora-
tion lime mortars and decay by-products in the Medita-
tion area of the Machu Picchu archaeological site.
20
In the Caribbean, there are no known studies on his-
torical mortars from the 16
th
century, although the first
mortars were made in the West Indies with the European
technology because the indigenous people of these is-
lands did not know about it and it was the European
conquerors and colonizers who introduced it. The first
constructions with mortar were made during Columbus’
Second Voyage in 1493, in the city of Isabela, on the is-
land of Hispaniola. Then, between 1494 and 1495 a se-
ries of fortifications were founded in the interior of the
island, among them La Concepción de la Vega. Around
it, the first mining town in America was established,
which was later destroyed by an earthquake and aban-
doned. In this village a fortification of bricks and lime
mortar was built that still includes the original materials
to be studied. For these reasons the aim of this research
is to characterize the mortar and plasters of the fortress
of Concepcion de La Vega, built at the beginning of the
16
th
century on the Hispaniola Island. The analysis is
based on optical microscopy (OM), Fourier transform in-
frared spectroscopy (FTIR), Raman spectroscopy and
thermogravimetric differential thermal analysis
(TG-DTA).
1.2 Fortress of Concepción de La Vega
In 1502 Nicolás de Ovando arrived to the island as
the governor of the territories discovered up to that mo-
ment. He had orders to occupy all the island’s territory
and established several cities. He brought many masons
with him for building works, as well as some construc-
tion materials such as nails, wooden beams and bricks.
The town of Concepcion de la Vega was established in
1494 but was relocated in 1504 about 2 leagues away
from the original site by Governor Ovando, to the current
location of the ruins. The city had a fortress whose con-
struction began around 1511 and was completed a few
years later, a gold foundry, a church that later became the
cathedral, several houses and a monastery. In 1562 an
E. PRIETO-VICIOSO et al.: CHARACTERIZATION OF LIME MORTAR AND PLASTERS OF FORTRESS CONCEPCION ...
534 Materiali in tehnologije / Materials and technology 56 (2022) 5, 533–539
Figure 1: Current state of the tower

earthquake destroyed the city and it was moved again, to
the current location. When the city and the fort were
abandoned, the site currently known as "Vega Vieja" was
used as a "brick quarry" to construct new buildings in the
new settlement of the city. The Church of Santo Cerro,
built at the end of the 19
th
century, on the outskirts of the
old city, was constructed using the bricks extracted from
the ruins of the fortress of La Concepción de La Vega.
The fortress of the Conception was a rectangular en-
closure of approximately 44m×21m,with brick walls
of approximately 1.67 m in width (2 varas castellanas)
and two cylindrical towers with walls of 1.75 m in width
placed diagonally opposite each other (Figure 1).
The existing tower has an outer diameter of 8.95 m,
an inner diameter of 5.35 m and more than 4-m high,
built-in brick masonry with 6 flared loopholes. The for-
tress had in its interior a tower of two levels that served
as the residence of the warden and other dependencies.
Today only one of the towers, parts of the outer wall and
parts of the walls of Torre del Homenaje remain (Fig-
ure 2).
2 EXPERIMENTAL PART
The analysis was performed on two samples that
were taken from the ruins of the fortress tower of
Concepción de La Vega: F1 is a mortar sample and F2 is
a plaster sample (Figure 3). The techniques used were:
• Optical microscopy (OM)
A general view of the samples was provided by anal-
yses with a Nikon (SMZ800N) stereomicroscope.
• Fourier transform infrared spectroscopy (FTIR)
FTIR measurements were performed by means of a
Bruker Vertex 70V spectrophotometer, in a range of
400–4000 cm
–1
. The samples were prepared with the
KBr pellet method (100 g sample/400 g KBr) in vacuum
desiccators under a pressure of 1.33 Pa (0.01 torr).
E. PRIETO-VICIOSO et al.: CHARACTERIZATION OF LIME MORTAR AND PLASTERS OF FORTRESS CONCEPCION ...
Materiali in tehnologije / Materials and technology 56 (2022) 5, 533–539 535
Figure 2: Current state of the fortress
Figure 3: Location of the samples

• Raman spectroscopy
In this study, Raman spectra were obtained using a
RM 2000 Renishaw equipped with a Leica microscope.
The excitation source was a laser emitting at 633 nm.
The laser output power was 25 mW. The spectra were
obtained in the 400–4000 cm
–1
range, with a resolution
of4cm
–1
. The acquisition time was 10 s, and 5 acquisi-
tions were performed to improve the signal/noise ratio.
The equipment was calibrated with the ± 520.6 nm band
of Si. The utilization of Raman provided valuable under-
standing of the chemical and physical properties of the
mortars and plaster.
• Thermogravimetric differential thermal analysis
(TG-DTA)
Thermal gravimetric analyses (TG-DTA) were car-
ried out with Q600 TA instruments that measure the heat
flow and weight changes in a sample as a function of
temperature (or time) under a controlled atmosphere.
The samples were heated from ambient temperature over
a range of 25–1000 °C at a heating rate of 10 °C/min and
nitrogen was used as the purging gas at a flow rate of
0.833 mL/s (50 mL/min).
All these analyses are compatible and complemen-
tary.
3 RESULTS AND DISCUSSION
3.1 Optical microscopy
Figure 4 shows a general view of the samples. In the
case of mortar F1 (Figure 4a) small black points indicate
the presence of the aggregate with a very low size.
Plaster F2 (Figure 4b) shows red particles that can
indicate the presence of iron oxide.
3.2 Fourier transform infrared spectroscopy
Figures 5 and 6 show the FTIR of mortar F1 and
plaster F2, respectively. The mortar sample shows the
following main characteristics: vibration bands of the
CO
3
2–
group present in calcite, a strong band at
1431 cm
–1
from stretching vibrations, as well as two nar-
row bands from bending vibrations
21
at 870 cm
–1
and
712 cm
–1
. Additionally, small bands from kaolinite at
(1030, 1077 and 1117) cm
–1
were identified.
22
Signals
due to the presence of organic matter probably coming
from contamination were also observed, as well as a
small signal at 1387 cm
–1
due to the presence of nitrates.
The plaster sample also shows calcite and kaolinite;
however, for this sample the bands from kaolinite have a
higher intensity than for the mortar.
3.3 Raman spectroscopy
The Raman spectrum of the plaster (F2) is shown in
Figure 7a, where the main bands can be attributed to
iron oxide in the form of hematite (a-Fe
2
O
3
) and there is
E. PRIETO-VICIOSO et al.: CHARACTERIZATION OF LIME MORTAR AND PLASTERS OF FORTRESS CONCEPCION ...
536 Materiali in tehnologije / Materials and technology 56 (2022) 5, 533–539
Figure 4: General view of the samples: a) mortar (F1), b) plaster (F2)
Figure 5: FTIR of the mortar (F1): C – calcite, K – kaolinite, OH –
OH from water molecules, N – nitrates, OMt – organic matter
Figure 6: FTIR of the plaster (F2): C – calcite, K – kaolinite, OH –
OH from water molecules, Q – quartz

a sharp band at 1085 cm
–1
indicating CO
3
2-
present in cal-
cite (CaCO
3
). The spectrum also shows a signal at
668 cm
–1
whose origin is uncertain. Bikias et al. and
other authors associate it with the Al-O-Si bond in
kaolinite,
23
while Aguayo et al. and some other authors
assign it to magnetite, an iron oxide present in igneous
and metamorphic rocks.
24
In the case of mortar (F1), only signals indicating
calcite are identified (Figure 7b).
Figure 8 shows the Micro-Raman spectra of two dif-
ferent aggregates of the mortar (F1), showing that both
calcite and quartz were used.
3.4 Thermogravimetric differential thermal analysis
In order to determine the amount of calcite present in
the mortar (F1), a DTA-TG was performed and the re-
sults are presented in Figure 9 and Table 1. The mortar
E. PRIETO-VICIOSO et al.: CHARACTERIZATION OF LIME MORTAR AND PLASTERS OF FORTRESS CONCEPCION ...
Materiali in tehnologije / Materials and technology 56 (2022) 5, 533–539 537
Figure 8: Micro-Raman spectra of the aggregates present in the mor-
tar sample (F1) (C – calcite, Q – quartz)
Figure 9: DTA-TG analysis of the mortar (F1)
Figure 7: Micro-Raman spectra of the samples: a) plaster (F2), b) mortar (F1) (C – calcite, H – hematite)

sample (F1) shows seven endothermic peaks. In ranges
of 70–130 °C and 110–180 °C, the weight loss due to
water of the crystallization of calcium sulfate hemi-
hydrate and dihydrate, respectively, takes place.
25
The
peaks are very small so they are probably due to atmo-
spheric pollution. The two peaks in the interval of
200–500 °C are attributed to the goethite transformation
into hematite and dehydroxylation of kaolinite, respec-
tively. The main endothermic peak at 797 °C with a mass
loss of 41.69 % is attributed to the decarbonation of cal-
cium carbonate. Finally, the endothermic peak at 929 °C,
without any weight loss, is possibly due to the crystalli-
zation of the new high-temperature phases such as clay
minerals.
26
The weight loss in the interval of 600–800 °C
is 41.96 % of CO
2
, which corresponds to 95.4 % of
CaCO
3
. These data indicate that the main compound in
the mortar is calcium carbonate with small amounts of
goethite and kaolinite, which are probably impurities
from the calcite.
4 CONCLUSIONS
Through chemical and mineralogical analyses, the
lime mortar and plaster of the Fortress of Conception de
La Vega, the first mining town in America, was charac-
terized. As in most constructions, the selection of the raw
materials for the preparation of mortars was based on the
geology of the area. The analysis indicates that the
binder in the mortar is calcium carbonate, with the cal-
cium carbonate also being the aggregate. The small
amounts of gypsum and nitrates found can be from atmo-
spheric pollution.
The plaster is also formed with calcium carbonate but
with kaolinite and hematite as the additives.
Acknowledgment
This work was funded by FONDOCYT 2020,
MESCyT – Ministry of Higher Education, Science and
Technology, under grant number 2020-1-3B6-000001,
MorCal project "Development of a lime mortar for plas-
tering with fungicidal and biocidal characteristics", CSIC
in call I-COOP+2020, project reference COOPB20548,
and CalCar Project "Portable spectroscopic techniques
applied to the study of binders and lime plaster of the
Caribbean Heritage". Funding was also received from
the Regional Government of Madrid, (S2018/NMT-4372
TOP Heritage-CM Programme). The authors also appre-
ciate the aid of the CSIC PTI-PAIS network.
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Table 1: Weight losses of the mortar (F1) determined with TG
Temperature interval
(°C)
Mortar (F1) CO
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/H
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O ratio Reaction
25–200 0.513 33.6 hygroscopic water and calcium sulphate dehydration
200–600 0.638 –
goethite transformation into hematite, kaolinite
dehydroxylation
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