Analytica Chimica Acta 557 (2006) 373–379

Analytical characterisation of ancient mortars from the archaeologicalRoman city of Pollentia (Balearic Islands, Spain)

C. Genestar∗, C. Pons, A. MasDepartment of Chemistry, University of the Balearic Islands (UIB), 07122 Palma de Mallorca, Spain

Received 16 May 2005; received in revised form 20 October 2005; accepted 24 October 2005Available online 28 November 2005

Abstract

Analytical characterisation of historic mortars from the Roman city of Pollentia (Mallorca) has been carried out by means of thermal analysis(thermogravimetry (TG) and derivative thermogravimetry (DTG)), X-ray diffractometry (XRD) and Fourier transform infrared spectroscopy(FTIR).

The aim of this research is to provide useful information about the construction mode of the mortars which served for lining purposes in ductdrains, cisterns, swimming pools, flooring mortars and wall renderings. The reported results converge to reveal the hydraulic nature of the majorityo e chemicalc .©

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f the mortars used for several hundred years to cover the diverse needs of the inhabitants of Pollentia. A fair correlation between thharacteristics of the studied mortars and the results of ancient Roman mortars from other archaeological sites has been established2005 Elsevier B.V. All rights reserved.

eywords: Ancient mortars; Roman mortars; Analytical characterisation; Thermal analysis; X-ray diffractometry; Fourier transform infrared spectrosco

. Introduction

Pollentia, located in southern Alcudia on the northeast coastf Mallorca, was founded in 123 BC by Quinto Cecilio Metelond is nowadays considered the most important Roman archae-logical site in the Balearic Islands[1]. In the early times it wasreduced city centre which underwent a considerable urban

evelopment during the emperor Augustus times, growing toeach 12 ha. Its decay started about III AC century due to firesnd destruction of buildings.

In the present work, the mortars from several parts of theorum and the annexed residential quarter, named “Sa Portella”,re investigated in order to characterise their nature as well as totudy the technological aspects involved in the manufacturingrocesses of Roman mortars. In this sense, it is relevant to state if

he differences arise mainly from the various historical periods ofonstruction or from the purposes they served, imparting to theortars the properties required by their function in the building.Thermal analysis (thermogravimetry (TG) and derivative

hermogravimetry (DTG)), X-ray diffractometry (XRD) and

Fourier transform infrared spectroscopy (FTIR) have proto be the most useful techniques for the analytical studancient mortars[2–13]. The establishment of a possible colation between the chemical characteristics of the mortarsPollentia and other published results from Roman archaeocal sites would be of great interest.

Up to date[14], the knowledge of the ancient building teniques traditionally used in Mallorca has been generally bon visual observations and properties. However, the comtional parameters are very important from both the histoand scientific point of view. Thus, the main objective ofpresent experimental work is to reduce this lacuna and toduce background knowledge of ancient mortars from Mallo

2. Experimental

2.1. Instrumentation and operating conditions

FTIR spectra were recorded using a Bruker IFS 66 FTIR strophotometer. Thirty-two signal-averaged scans were acqon the samples. KBr (IR grade, Merck) pellets of powered s

−1

∗ Corresponding author. Tel.: +34 971 173258; fax: +34 971 173426.E-mail address: nina.genestar@uib.es (C. Genestar).

ples were examined in the 4000–400 cmregion at a resolutionof 4 cm−1. For the preparation of samples, 1–2 mg of the fractionmortar were mixed homogenously with 100 mg of anhydrous

003-2670/$ – see front matter © 2005 Elsevier B.V. All rights reserved.

oi:10.1016/j.aca.2005.10.058

374 C. Genestar et al. / Analytica Chimica Acta 557 (2006) 373–379

KBr in an agate mortar. A pressure of 10 t was applied to thismixture in order to obtain transparent pellets. Identification isbased on comparison of the bands of the recorded FTIR spectrawith those of reference materials or literature.

For thermogravimetric analysis (TG–DTG), samples weredried at room temperature (in dessecator with silica gel blue)for at least 48 h. The TG–DTG curves were obtained using athermobalance from TA instruments (SDT 2960) with temper-ature and weight precision of 0.1◦C and 0.1�g, respectively.The sample was varied between 5 and 10 mg and weighed onceramic pans. TG–DTG experiments were performed in flow-ing dry nitrogen atmosphere (100 ml min−1) at a heating rate of10◦C min−1 within the temperature range of 25–1000◦C.

XRD analysis was performed on a Siemens D5000 powderdiffractometer equipped with a primary beam monochromatorand Cu K� radiation. The step size used was 0.050A (withinthe angle range of 3–60◦). The step time was established in 2 s.

2.2. Sampling

Two well-defined areas were selected for sampling belongingto two distinctive historical periods of the city of Pollentia (I BCand III AC, respectively). The first selected area correspondsto the Forum and the second was the residential quarter knownas “Sa Portella”, which comprises several residences (such asthe so-called “La Casa dels Dos Tresors” and “Casa del Cap deB

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Table 1Sampling and location of the Pollentian mortars

Sample Kind of mortar and location Sampling area

P-1.1 Lining mortar external, cistern Forum, E18P-1.2 Lining mortar internal, cistern Forum, E18P-2 Flooring mortar Forum D18P-3 Flooring mortar Forum, D19P-4 Lining mortar, duct drain Forum, F 18P-5 Flooring mortar Forum, H18P-6 Flooring mortar Forum, J18P-7 Flooring mortar Forum, J15P-8 Flooring mortar Forum, K15P-9 Deposit of raw material Forum, K14P-10 Lining mortar external, cistern Forum, J13P-11 Flooring mortar Forum, K13P-12 Lining mortar, swimming pool Forum, K13P-13 Lining mortar, from the tower Forum, J14P-14 Leveller stuffing mortar (from

theForum)Forum, J14

P-15 Lining mortar external Forum, L16P-16 Flooring mortar Forum, H22P-17.1 Plaster mortar, from the wall Forum, J20P-17.2 Lining mortar internal of P-17

sampleForum, J20

P-18 Plaster mortar, from the wall Forum, I20P-19 Deposit of raw material Forum, J21P-20 Flooring mortar Forum, E10P-21 Lining mortar, inner wall Forum, F10P-22 Lining mortar, external wall Forum, H11P-23 Lining mortar Forum, J11P-24 Flooring mortar “Cap de Bronze”

house, Sa PortellaP-25 Plaster mortar, inner wall “Cap de Bronze”

house, Sa PortellaP-26 Flooring mortar “Cap de Bronze”

house, Sa PortellaP-27 Flooring mortar “Cap de Bronze”

house, Sa PortellaP-28 Plaster mortar, inner wall “Dos Tresors” house,

Sa PortellaP-29 Flooring mortar “Dos Tresors” house,

Sa PortellaP-30 Plaster mortar, inner wall “Dos Tresors” house,

Sa Portella

such as hardness and cohesion of the final product. Naked eye ormagnifying glass macroscopic examination of the tested sam-ples revealed, in general, high aggregate/matrix cohesion.

Chemical characterisation of the main molecular componentswas performed by means of FTIR, XRD—in order to identifythe crystalline structure of the mortar components—and thermalanalysis (TG–DTG) analysis.

The grain size distribution is the first step in the methodol-ogy to analyse historic mortars, thus, information on the differentfractions present in the mortars and their mixture ratio duringmortar preparation was obtained. The results of the fractionationand sieving of the mortars samples were represented as the wt.%of each particle-size range against particle-size range. Two ten-dencies were observed in the granulometric analysis: namely,symmetric and descending distributions. The two types of grainsize distribution are displayed inFigs. 3 and 4a and b. In general,the descending distribution (Fig. 3) belongs to flooring mortars,

ronze”).Sampling was accomplished in conjunction with the arc

logists and performed on the basis of historical and archonic considerations. Information regarding sampling locand architectural use are provided inTable 1. Figs. 1 and 2show

he plan of the Roman city of Pollentia with the corresponampling locations.

The state of conservation of the samples characteriseood.

.3. Analytical methodology

The granulometric analysis of samples by mechanicalng (ISO 565 series sieves, meshes of 4, 2, 1, 0.5, 0.25.063 mm of diameter) was carried out in order to obtain ination about their grain size distribution and an estimatio

he proportions of binder/aggregate within the mortar. Thear sample, about 100 g, was fractionated in a column of stirred for ca. 30 min, and the masses of the colleted fracere determined. The most significant granulometric frac

or the aim of this research, is that of particle size <63�montaining the binder. Next, the fine particle size <63�m wasnalysed by FTIR, XRD and thermal analysis (TG–DTG).

hermore, treatment with 2 mol l−1 hydrochloric acid was carrieut in order to determine the insoluble residue. The methodo

ollowed has been previously described elsewhere[14].

. Experimental results and discussion

The nature and composition of raw materials in the manuure of mortars contribute to a large extent to relevant prope

C. Genestar et al. / Analytica Chimica Acta 557 (2006) 373–379 375

Fig. 1. Plan of theforum of Pollentia. Sampling areas.

whereas the symmetric distribution (Fig. 4a and b) happenedto be related to the lining and plaster mortars. A considerableamount of fragments with a diameter greater than 4 mm can befound in all the flooring mortars (granulometric distributions of

several flooring mortars are shown inFig. 3). Different sym-metric distributions were found in the lining and plaster mortarsanalysed. Thus, unimodal distribution around 2 mm (P-1.1, P-10) and 1 mm (P-23) particle-size range can be seen inFig. 4a.Bimodal distribution around 2 and 0.5 mm particle-size range(P-12, P-13 samples) and around 0.5 and 0.063 mm (P-15 sam-ple) is represented inFig. 4b. On the other hand, in all the samplesanalysed, the finest particle size (<63�m) containing the binderrepresents less than 10% of the whole sample.

The FTIR spectra of analysed particle-size fraction <63�mshow characteristic bands of calcium carbonate (1430, 873, and712 cm−1) as well as the IR band at 3436 cm−1 due to freehydroxyl ions of water in all the samples reported. Resultsobtained allow us to distinguish between three types of bindercomposition. The following samples P-1.1, P-1.2, P-9, P-10, P-

Fig. 2. Plan of the “La Portella” of Pollentia and sampling points.

Fig. 3. Grain size distribution of flooring mortar.

376 C. Genestar et al. / Analytica Chimica Acta 557 (2006) 373–379

Fig. 4. Grain size distribution of lining mortars: (a) unimodal distribution and(b) bimodal distribution.

11, P-12, P-13, P-20, P-22, P-23, P-25, P-27 and P-29 showtwo characteristic peaks (in addition to the presence of cal-cium carbonate bands) attributable to silicates, i.e. the SiO Siband at 1030 cm−1 and the O M O at 460 cm−1. P-5, P-21 and P-28 samples are practically composed of carbonate,exclusively; only a slight shoulder at 1020–1030 cm−1 wasdetected. The remaining samples happen to be composed ofcarbonate (1430, 873, and 712 cm−1), silicate (Si O Si bandat 1029–1032 cm−1) and iron oxides (535 and 470 cm−1). TheFTIR spectra from the three types of binder samples are dis-played inFig. 5.

F ) P-4s

Table 2Mineralogical composition of the <0.063 mm fraction by DXR analysis

Sample Calcite Quartz

P-1.1 *** *P-1.2 *** *P-2 *** trP-3 *** trP-4 *** trP-5 *** trP-6 *** **P-7 *** trP-8 *** trP-9 *** –P-10 *** **P-11 *** *P-12 *** *P-13 *** –P-14 *** *P-15 *** trP-16 *** **P-17.1 *** **P-17.2 ** ***P-18 *** trP-19 * ***P-20 *** *P-21 *** –P-22 *** *P-23 *** –P-24 *** trP-25 *** trP-26 *** trP-27 *** trP-28 *** trP-29 *** trP-30 *** tr

The number of asterisks is related to the relative abundance; tr: mineral in traceamount.

The results of the XRD analysis (seeTable 2) indicate thatcalcite is the main mineralogical constituent of all the mor-tars, except for P-19 and P-17.2 samples. These samples weresiliceous in nature. In addition, the presence of quartz as minor-ity component or even at trace levels was also detected.

Considerably, variable quantitative results for the acid insol-uble fraction were obtained after HCl treatment. In this way, agood correlation with FTIR analysis was found. Thus, P-5, P-21 and P-28 samples, composed mainly of calcium carbonate,present the lowest acid insoluble residue content. The presenceof silicon dioxide (or insoluble silicate) after HCl treatment wasconfirmed by FTIR.

TG–DTG analysis is used as a useful tool to characterise his-toric mortars, since it easily detects the presence of compoundsof hydraulic characteristics and provides the fundamental infor-mation which allows the identification of the type of mortar.Table 3reports the percentage of weight loss estimated fromthe TG–DTG curves within the selected temperature ranges. Inthe temperature range from 30 to 120◦C the weight loss is dueto adsorbed water, from 120 to 200◦C the weight loss of waterfrom hydrated salts occurs, between 200 and 600◦C the weightloss is due to structurally bound water from the hydrauliccompounds and, finally, the loss of CO2 as a consequence of

ig. 5. FTIR spectra of the three kinds of mortars. (a) P-12 sample; (bample; (c) P-21 sample.

C. Genestar et al. / Analytica Chimica Acta 557 (2006) 373–379 377

Table 3TG–DTG weight losses as a function of the temperature range (wt.%)

Sample 30–120◦C 200–600◦C 600–800◦C

P-1.1 1.7 4.8 22.3P-1.2 3.3 5.1 20.1P-2 1.2 4.5 31.9P-3 1.1 3.7 33.9P-4 2.1 4.8 35.3P-5 0.7 3.5 36.1P-6 1.7 4.8 18.3P-7 0.8 2.9 29.9P-8 1.2 3.9 29.4P-9 1.7 4.8 31.6P-10 3.5 5.1 18.9P-11 2.1 4.3 30.7P-12 2.6 6.3 27.9P-13 1.2 4.8 34.1P-14 0.9 1.4 34.6P-15 0.7 2.3 37.9P-17.1 1.6 3.3 30.6P-17.2 1.6 2.7 14.1P-18 1.0 2.6 34.7P-19 1.2 2.9 11.6P-20 1.3 4.2 27.8P-22 1.0 4.2 31.4P-23 0.9 3.0 36.1P-24 0.8 4.0 33.2P-25 1.7 4.9 31.3P-26 0.5 3.0 33.7P-27 2.2 4.3 21.4P-28 0.9 4.9 34.8P-30 0.9 4.4 33.9

the decomposition of calcium carbonate (CaCO3) takes placeat temperature range between 600 and 800◦C.

The term hydraulic refers to two specific properties: the prop-erty of hardening when water is added to the dry binder, andalso the capacity to harden under water. The hydraulic com-pounds are obtained from the reactions of Ca(OH)2 with naturalearths of volcanic source or artificial pozzolanas, such as groundfired bricks and tiles or ceramic shreds used when natural poz-zolanic materials are not available. Natural pozzolan containssilicon dioxide in amorphous state as well as aluminium andiron hydrated oxides may be contained in the natural or artificialpozzolans[9,13]. The presence of aluminium and iron hydratedoxides together with the lime binder contributes to the mortarhydraulic character[2–4,6,7,9]. The so-called hydraulic mor-tars include all materials with an amount of structurally boundwater to the hydraulic components higher than 3%, whereatypical lime mortars are characterised by less than 3% of structurally bound water to the hydraulic components (the so-called

Fig. 6. CO2 to structurally bound water ratio in relation to % CO2 for groupsA, B, C, D and raw materials (P-9 and P-19).

non-hydraulic mortars)[6,9,10,13]. In this way, only the mor-tar samples P-7, P-14, P-15 and P-18 are of non-hydraulicnature.

The CO2 to structurally bound water ratio in relation toCO2 percentage (% weight loss in the temperature range of600–800◦C) is shown inFig. 6. The inverse trend of hydraulic-ity of mortars is being augmented exponentially with CO2.Thisrepresentation allows a good classification of the mortar nature[6,9,13]. From the observation of this plot several groups ofmortars can be discerned. Group A with a percentage of CO2between 10 and 22.5% and CO2/H2O ratio below 5. The sec-ond group with a percentage of CO2 between 27.5 and 35% andCO2/H2O ratio between 5 and 10, named Group B. Group C witha percentage of CO2 surpassing 35% and CO2/H2O ratio over10. Group D is constituted by mortars of non-hydraulic nature,characterized by a percentage of CO2 and CO2/H2O ratio sim-ilar to group C but with a weight loss within the temperaturerange of 200–600◦C lower than 3%.

The main chemical characteristics from the thermogravi-metric analysis are summarized inTable 4. Distinction wasmade among the four groups with different statistical results.Group A is composed of P-1, P-6, P-10, P-12, P-17-2, P-19 andP-27 samples. Samples P-2, P-3, P-4, P-8, P-9, P-11, P-13, P-16, P-17-1, P-20, P-22, P-24, P-25, P-28 and P-30 constituteGroup B. Group C is formed by P-5, P-21, P-23, P-26 and P-29 samples. Group D comprised samples P-7, P-14, P-15 andP

isp ortarsb car-b ction( nate

Table 4Chemical characteristics of historic mortars from Pollentia

Group Adsorbed water (%) Structu

A (n = 7) 1.9± 0.5 5.1± 0.B (n = 14) 0.7± 0.2 4.3± 0.C (n = 5) 0.4± 0.1 3.3± 0.D non-hydraulic (n = 4) 0.3± 0.1 2.3± 0.

R

esults are expressed as the mean± standard deviation.

s-

-18.In Fig. 7, the calcium carbonate/acid insoluble fraction

lotted versus the calcium carbonate percentage. The melonging to group A show low percentages of both calciumonate (25–50%) and calcium carbonate/acid-insoluble fra0.5–2.5). Group B was characterised by a calcium carbo

rally bound water (%) CO2 (%) CO2/H2O ratio

5 21.5± 3.5 4.3± 0.55 31.9± 2.4 7.5± 0.83 35.7± 1.6 10.8± 0.76 34.2± 3.3 16.0± 5.8

378 C. Genestar et al. / Analytica Chimica Acta 557 (2006) 373–379

Table 5Chemical characteristics of historic mortars found in the literature

Mortar type Adsorbed water (%) Structurally bound water (%) CO2 (%) CO2/H2O ratio Reference

Typical lime <1 <3 >32 10a, 7.5–10b [6,13]<1 1.1–1.6 31–38 23–29 [9]

Hydraulic lime >1 3.5–6.5 24–34 4.5–9.5 [6,13]>1 4.1–6.1 27–34 4.3–7.9 [9]

Hydraulic lime with unaltered portlandite >1 4–12 18–34 1.5–9 [6,13]

Artificial pozzolanic 1–4 3.5–8.5 22–29, 10–19c 3–6 [6,13]1–1.8 4.1–4.9 23.5–25.3 5.3–5.9 [9]

Natural pozzolanic 4.5–5 5–14 12–20 <3 [6,13]1.6–3.2 7.6–11.8 17.6–20 1.3–2.4 [9]

a Aggregates of calcareous nature.b Aggregates of silicoaluminate nature.c Byzantine “concrete”.

content between 65 and 75% and the calcium carbonate/acid-insoluble fraction comprised between 2 and 5. Group C hada calcium carbonate percentage of 76–86%, and a higher cal-cium carbonate/acid-insoluble fraction (between 4 and 10) thangroups A and B. Group D, formed by the mortars of non-hydraulic nature, exhibited a wide range of calcium carbon-ate content (68–86%) and the calcium carbonate/acid-insolublefraction comprised between 3 and 6.

In order to know the nature of the aggregates, the size frac-tion between 1 and 2 mm was analysed by FTIR. The anal-ysis showed the presence of carbonate and silica or silicatefor mortars belonging to groups A and B. The aggregates ofthe mortars from group C were composed of calcium carbon-ate as a major component and silicate as trace compound. Theaggregates from group D were composed exclusively of calciumcarbonate.

The analysis of the raw material found at the archaeologicalsite (samples P-9 and P-19) shows very different results. TheFTIR spectrum of P-9 sample revealed the presence of calciumcarbonate together with small amounts of silicate (weak signalsat 1066 and 617 cm−1). On the other hand, in FTIR spectrumof P-19 sample, besides the presence of carbonate bands (1432,875 and 712 cm−1), a very intense band of silicates (1030 cm−1)and iron oxides (530 and 471 cm−1) were found. The charac-terisation by means of XRD analysis revealed the presence of

FA

calcite in sample P-9 and quartz as majority and calcite as minor-ity compounds in sample P-19. When comparing structurallybound water to the hydraulic components, P-9 happens to con-tain larger amounts in relation to P-19 sample. Furthermore,from the TG–DTG analysis it was deduced a calcium carbonatepercentage of 72% for P-9 sample against 26% correspondingto P-19 sample.

The results obtained enabled to assign group A as artificialpozzolanic mortars, group B as hydraulic lime mortars withaggregates of siliceous nature and group C as hydraulic limemortars with aggregates of calcareous nature. Samples of groupD are typical lime mortars of non-hydraulic nature. According tothis classification, the raw materials (P-19 and P-9) are includedinto the groups A and B, respectively (Fig. 6).

By comparing the experimental results (reported inTable 4)with existing literature data (seeTable 5) a good correlation wasfound.

Artificial pozzolanic mortars (group A and seeTable 1) weremainly found in cisterns, duct drains, swimming pools as effi-cient waterproofing materials with lining purposes on the innerwalls. The main characteristics of their structure are the presenceof bricks in the form of ceramic fragments or ceramic power, aspozzolanic additives in the matrix of the aggregates.

4. Conclusions

inat-i ain)r es tot

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ig. 7. CaCO3 to insoluble HCl residue ratio in relation to % CaCO3 for groups, B, C, D and raw materials (P-9 and P-19).

The physico-chemical characterisation of mortars origng from the Roman city of Pollentia (Balearic Islands, Speveals differences in the mortars employed and contributhe knowledge of the Roman construction mode.

From the granulometric distribution, differences are fomong flooring mortars and those which served for linurposes in duct drains, cisterns, swimming pools and whus, a descending distribution happened to correspoooring mortars, whereas lining and plaster mortars ex

ted a symmetric distribution. The aggregate/binder ratioeight is higher in flooring mortars than lining and plaortars.FTIR analysis of the 63�m fraction indicates the existen

f three types of binders: the first containing calcium carbo

C. Genestar et al. / Analytica Chimica Acta 557 (2006) 373–379 379

and silicates, the second composed of carbonate, silicates andvariable amounts of iron oxides and a third with the presence ofcarbonates and low amounts of silicates.

Thermal and microchemical investigation results reveal thehydraulic nature of most of the mortars used for several cen-turies to cover the needs of the inhabitants of Pollentia. From 30samples analysed, only four happened to be lime mortars pre-senting non-hydraulic properties. The obtained results enablethe classification of the mortars studied into four categories:artificial pozzolanic mortars (group A), hydraulic lime mortars(group B and group C, with aggregates of siliceous and cal-careous nature, respectively) and the typical lime mortars ofnon-hydraulic nature (group D).

Different kinds of raw materials were used. From the analyt-ical data of the samples P-19 and P-9 it may be concluded thatthey constitute the raw material for the manufacture of the arti-ficial pozzolanic mortars (group A) and hydraulic lime mortarswith aggregates of siliceous nature (group B).

A correlation between chemical characteristics of the mor-tars studied with published results of ancient Roman mortarsfrom other archaeological sites was attained. The principalcomposition differences are related to the purpose the mortarsserved, imparting to the mortars the properties required by theirfunction in the building. Thus, the lining mortars from depositsand swimming pools are those presenting the best hydraulicproperties.

thes i.e.I iquea fouc

tiona manb on ot

Acknowledgements

Financial support through “Mecanismes de Participacio deInvestigadors” provided by Govern Balear is gratefully acknowl-edged. The authors would also like to thank Dra. M. Orfila fromthe Universidad de Granada for providing the excavation sam-ples for this work and the Serveis Cientıfico-tecnics (SCT) de laUniversitat de les Illes Balears (UIB).

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[ ini,

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[ om-

[

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In conclusion, the results provide interesting informabout the technological knowledge of the ancient Rouilders, such as the techniques involved in the preparatihe binding materials used for various purposes.

r

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