Caratterizzazione mineralogica e strutturale di malte e intonaci del sito archeologico di Barsinia, Giordania settentrionale
10.6092/issn.1973-9494/4742
Summary Twelve mortar and plaster samples excavated in the archaeological site of Barsinia were mineralogically and petrographically examined by XRay Diffraction (XRD) and Stereo and Polarized Light Microscopy, while the total carbonate content was measured using a DietrichFruhling Calcimeter. The physical properties of the samples, such as water uptake under atmospheric pressure and under vacuum, together with density and porosity, were measured. Only twelve samples were available for the purposes of this study: 8 plaster samples and 4 mortar samples. Eleven samples out of the total number of samples were mortars or plasters with lime binder and silica aggregate; calcite and quartz were identified in all of these samples. In most of the samples one or more pozzolanic components were detected; a hydraulic effect therefore exists in practically most of the studied mortars. Excluding the plasters taken from waterbearing constructions such as cisterns, and the mortar sample from the compact floor, the binder content is high; in general, the overall porosity of the studied samples is high. Porosity and petrographic investigation results suggest that the burning temperature of the limestone was low and/or the duration of the combustion was short; such preparation conditions produce a desirable quicklime. Owing to the significant compositional and textural differences between the samples that were reported, there is consequently no suitable general mortar that can be adopted for the restoration of the whole site.Riassunto Dodici campioni di malta e intonaco, prelevati dal sito archeologico di Bar sinia, sono stati esaminati mineralogicamente e petrograficamente utilizzando l’analisi di diffrazione a raggi X (XRD) e microscopi stereoscopici e a luce pola rizzata, mentre il contenuto totale di carbonati è stata misurato utilizzando il cal cimetro DietrichFruhling. Sono state misurate le proprietà fisiche dei campioni, come l’assorbimento di acqua a pressione atmosferica e sotto vuoto, insieme alla densità e alla porosità. Per le finalità di questo studio erano disponibili solo dodici campioni: 8 campioni di intonaco e 4 campioni di malta. Undici campioni rispetto al numero totale erano malte o intonaci con legante di calce e aggregati di silice, e in tutti questi campioni potrebbero essere identificati calcite e quar zo. Nella maggior parte dei campioni sono stati rilevati uno o più componenti pozzolanici e, dunque, l’effetto idraulico si verifica praticamente nella maggior parte delle malte studiate. Escludendo gli intonaci prelevati da costruzioni ac quifere quali cisterne e il campione di malta dal pavimento compatto, il conte nuto di legante è alto. In generale, la porosità dei campioni studiati è alta. La porosità e i risultati dell’indagine petrografica suggeriscono che la combustione del calcare è avvenuta a temperature basse e/o la durata di combustione è stata breve; tali condizioni di preparazione producono la calce viva. Sarebbero state riportate significative differenze compositive e tessutali tra i campioni e, pertanto, non può essere impiegata nessuna generale malta di composizione per il restauro dell’intero sito.Résumé Douze échantillons de mortier et d’enduit prélevés du site archéologique de Barsinia ont été analysés d’un point de vue minéralogique et pétrographique par analyse par diffraction de rayons X (DRX) et au microscope stéréoscopique et à la lumière polarisée. La teneur totale en carbonates a été mesurée par le cal cimètre de DietrichFruhling. Les propriétés physiques des échantillons ont été mesurées, par ex. l’eau absorbée à la pression atmosphérique et sous vide, la densité et la porosité. Pour cette étude, nous n’avions que douze échantillons: 8 échantillons d’enduit et 4 de mortier. Onze échantillons sur douze étaient des mortiers ou des enduits avec un liant de chaux et des agrégats de silice. La calcite et le quartz pourraient être identifiés dans la totalité des échantillons. Dans la plupart des échantillons, on a détecté un ou plusieurs composants de type pouzzolanes. Dès lors, l’effet hydraulique se vérifie pratiquement dans la plupart des mortiers étudiés. La teneur en liant est élevée. Font exception les enduits prélevés de constructions aquifères (par ex., citernes) et l’échantillon de mortier prélevé du sol compact. En général, les échantillons étudiés étaient très poreux. La porosité et les résultats de l’étude pétrographique font supposer une combustion courte du calcaire, et/ou une combustion à basse température, conditions de préparation qui sont celles de la chaux vive. Du fait des différences importantes de composition et de texture qui auraient été constatées entre les échantillons, aucun mortier de composition standard ne peut être utilisé pour restaurer l’ensemble du site.Zusammenfassung Zwölf Mörtel und Putzproben aus der archäologischen Ausgrabungsstätte von Barsinia wurden mineralogischen und petrografischen Untersuchungen mittels Röntgenbeugung (XRD) und Einsatz von StereoPolarisationsmikroskopen un terzogen, während der GesamtKarbonatgehalt mithilfe eines Calcimeters nach DietrichFrühling ermittelt wurde. Gemessen wurden die physikalischen Eigen schaften der Proben, wie Wasserabsorption bei Atmosphärendruck und unter Va kuum, sowie Dichte und Porosität. Für diese Studie standen nur zwölf Proben zur Verfügung: 8 Putz und 4 Mörtelproben. Von allen vorhandenen Proben bestan den elf aus Mörtel oder Putz mit Kalkbinder und Kieselerde als Zuschlagstoff und in allen Proben könnten Calcit und Quarz nachgewiesen werden. In den meisten Proben wurden eine oder mehrere PuzzolanKomponenten ermittelt, d. h. die Bindung von Wasser findet praktisch in den meisten der untersuchten Mörtel statt. Von den aus Wassergewerken wie beispielsweise Zisternen stammenden Putzproben und den Mörtelproben aus dem kompakten Bodenbelag abgesehen, ist der Bindemittelgehalt hoch. Generell weisen die untersuchten Proben hohe Porosität auf. Die Porosität und die Ergebnisse der petrografischen Analyse las sen darauf schließen, dass die Verbrennung des Kalks bei niedrigen Temperatu ren stattgefunden und/oder dass diese Verbrennung nur kurze Zeit gedauert hat. Unter derartigen Herstellungsbedingungen entsteht Branntkalk. Zwischen den Proben wurden bedeutende Unterschiede in der Zusammensetzung und Gewe bestruktur festgestellt, daher ist die Verwendung eines Mörtels mit allgemein ge eigneter Zusam mensetzung für die Restaurierung des gesamten Standorts nicht möglich.Resumen Doce muestras de mortero y enlucido, tomadas en el yacimiento arqueológico de Barsinia, han sido examinadas desde el punto de vista mineralógico y petrográfico mediante análisis de difracción de rayos X (XRD) y microscopios estereoscópicos y de luz polarizada, mientras que el contenido total de carbonatos se ha medido empleando el calcímetro DietrichFruhling. Se han medido las propiedades físicas de las muestras, como la absorción de agua a presión atmosférica y al vacío, así como también la densidad y la porosidad. Para los fines de este estudio solo se disponía de doce muestras: ocho de enlucido y cuatro de mortero. Del total de las muestras, once estaban constituidas por morteros o enlucidos con aglutinante de cal y agregados de sílice. En todas ellas se han detectado calcita y cuarzo. En la mayoría se ha hallado por lo menos un componente puzolánico, por lo que puede afirmarse que en gran parte de los morteros estudiados se da el efecto hidráulico. A excepción de los enlucidos tomados en construcciones acuíferas, como cister nas, y de la muestra de mortero del suelo compacto, el contenido de aglutinante es elevado. En general, la porosidad de las muestras estudiadas es alta. La porosi dad y los resultados del estudio petrográfico sugieren que la combustión de caliza fue de breve duración y/o tuvo lugar a bajas temperaturas; dichas condiciones de preparación producen cal viva. Como se han encontrado diferencias significativas en la composición y los tejidos de las muestras, no se puede emplear ningún mor tero de composición de tipo genérico para restaurar la totalidad del yacimiento.简介 针对十二份取自 Barsinia 建筑的泥浆和灰泥样本，均使用X射线衍射、立体显微镜和 偏光显微镜进行矿物学和岩相学分析测试，总含碳量使用 DietrichFruhling 碳酸计进行 测量。针对样本的物理特性，进行了如压力环境和真空下吸水性，材料密度和多孔性 测试。为达到实验目的仅准备 12 份样本： 8 份灰泥（ Plaster ）样本， 4 份泥浆（ Mor tar ）样本。总样本中的 11 份灰泥或泥浆样本混有石灰粘合剂和氧化硅集合体，每份样 本中均有方解石和石英成分存在。 在大部分样本中存在一种或多种白榴火山灰成分，因此在大部分泥浆研究中液压作 用均被实际证实。排除从含水结构如蓄水池中获得的灰泥样本和紧凑地板结构中获得 的泥浆样本，其他样本中均有高含量的粘合剂成分。多孔性和岩相调查提醒石灰常温 燃烧性很低，并且/或着燃烧时间持续很短；这样的条件下产生生石灰。样品间组成和 组织成分有很明显差别，因此在进行整个建筑群修复时，不可以仅使用同一种泥浆。Резюме Двенадцать образцов раствора и штукатурки, отобранных в археологиче ских раскопках в Барсинии, стали предметом минералографического и петрог рафического исследования, используя рентгенофазовый анализ и стереоско пические и поляризационные микроскопы, в то время как общее содержание карбонатов было измерено при помощи кальциметра ДитрихаФрюлинга. Были измерены такие физические характеристики образцов, как поглощение воды при атмосферном давлении и в вакууме, а также их плотность и пористость. Для проведения этого исследования в распоряжении имелось только двенад цать образцов: 8 образцов штукатурки и 4 образца раствора. Из общего коли чества образцов одиннадцать представляли собой растворы или штукатурки с известковым вяжущим и кремнеземными агрегатами, и во всех этих образцах можно бы обнаружить кальцит и кварц. В большинстве образцов были найде ны один или несколько пуццолановых компонентов, поэтому, гидравлический эффект возникает практически в большинстве исследуемых растворов. За исключением штукатурок, отобранных в таких водоносных сооружениях, как цистерны, и образца раствора из плотного пола, наблюдается высокое содер жание вяжущего вещества. В общем плане пористость исследуемых образцов является высокой. Пористость и заключения петрографического исследования наводят на мысль о том, что известняк горел при низкой температуре и/или в течение непродолжительного времени. При таких условиях подготовки получа ется негашеная известь. Поскольку были обнаружены значительные различия в составе и в текстуре разных образцов, невозможно применение одного общего раствора для реставрации всего объекта.
application/pdf
1973-9494
4742
en
Lamia Salem EL-Khouri
Conservation Science in Cultural Heritage
conservation
Mineralogical and textural characterization of mortars and plasters from the archaeological site of Barsinia, northern Jordan
Text.Serial.Journal
https://conservation-science.unibo.it/
14
Articles
2014-12-20
2015-02-25
2014-12-20
2015-11-02
63-79
CSCH
Lamia Salem EL-Khouri
2014/12/20
10.6092/issn.1973-9494/4742
63
1973-9494
conservation
en
79
LUBICA W., 1996 (1), Study of salt-frost attack on natural stone. In: Riederer J, editor. 8th International Congress on Deterioration and Conservation of Stone, Berlin, pp. 563-571.
Mineralogical and textural characterization of mortars and plasters from the archaeological site of Barsinia, northern Jordan
https://conservation-science.unibo.it/article/download/4742/4246
14
M     INERALOGICAL AND TEXTURAL CHARACTERIZATION
      OF MORTARS AND PLASTERS FROM THE ARCHAEO-
      LOGICAL SITE OF BARSINIA, NORTHERN JORDAN


    Mustafa Mohammad AL-Naddaf•
    Department of Conservation and Management of Cultural Resources
    Faculty of Archaeology and Anthropology
    Yarmouk University, Jordan

    Lamia Salem EL-Khouri
    Department of Archaeology
    Faculty of Archaeology and Anthropology
    Yarmouk University, Jordan

    Keywords: Jordan, mortar, aggregate, physical properties, conservation

   1. Introduction

   Barsinia is located in the northwestern rural landscape of Jordan (Fig. 1), about 15 km
west of the modern city of Irbid. The site is currently surrounded by agricultural fields, where
cereals and olive trees are cultivated. The seasons of excavations, in 2006 and 2007, uncov-
ered many architectural remains and artifacts, including pottery, glass vessels, stone grinding
tools, and metal items, thus reflecting a flourishing settlement, particularly during the Hel-
lenistic, Roman, Byzantine and Umayyad periods (ca. 2nd century BC - 8th century AD) [1-4].




                                                                                                        CONSERVATION SCIENCE IN CULTURAL HERITAGE
   The site includes three main parts: the domestic structures, the cemetery, and the
agricultural fields. All the buildings were constructed for the most part using local lime-
stone, some of which was interbedded with thin layers of flint. Marble was found in
small quantities at the site, the most impressive pieces being a small cylindrical pillar
and fragments of a decorated marble slab with geometrical and floral carvings, prob-
ably part of a chancel screen from a Byzantine church.

   The walls were built using stones of different kinds and sizes. Both well-cut stones
and rubble stones were used in constructing the same wall, indicating different phases
of construction. Most of the walls were covered by plaster, as traces of it were still vis-
ible in some places (Fig. 2– plaster, Area A, Square B10).

   During the two seasons of excavations at the site, in 2006 and 2007, twelve sam-
ples of plasters and mortars were collected; eleven samples were found in 2006 and
only one sample (Br.07.B.A3.5) was found in 2007. The scarcity of the collected sam-
ples was due to the continued settlement, and disturbance and re-use of the residential
facilities throughout a period of approximately one thousand years; from the late Hel-
lenistic to early Islamic periods. The majority of the samples were found in the resi-
dential facilities, except sample Br.06.NecI.Tomb1.1, that was unearthed in a Roman-
Byzantine tomb and samples (Br.06.NecI.Tomb1.1, Br.06.A.A9.7a and Br.06.A.A9.7b)
that were originally parts of the plaster which covered the walls of a late Hellenistic/
early Roman cistern (1st century BC- 1st century AD) (Fig. 3).
                                                                                                   63
M. Mohammad AL-Naddaf, L. Salem EL-Khouri - Mineralogical and textural characterization of mortars and plasters




                                                                                                                          Figure 1. A map of Jordan showing the location
                                                                                                                          of Barsinia




                                                                                                                  Figure 2. The residential area at Barsinia, and the sampling sites




                                                                                                             64
   Historical lime mortar and plaster in Jordan have been the subject of a very
limited number of studies. Al-Saad and Abdel-Haim (2001) evaluated 3 types of
mortars to be used as a restoration mortar for the Qasr Al-Bint monuments in Petra.
The selection criteria was based on the mechanical and physical properties of the
tested mortars compared with that of the building stone [5]. Dunn and Rapp (2004)
studied Roman and Byzantine mortars and pozzolanic materials from the archaeo-
logical site of Umm al-Jimal; the studied samples were petrographically and miner-
alogically characterized [6]. Abde Hadi and Abdel Hadi (2012) studied lime mortar
and plaster in the historic castle of Al-Shawbak in Southern Jordan. The physical,
mechanical and chemical properties of the collected samples were determined; ac-
cordingly, restoration mortar and plaster were prepared from bituminous limestone
designed to rehabilitate the castle [7]. Bani Yaseen et al. (2013), analyzed Roman
mortar from the archaeological site of Jerash by using petrographical, mineral-
ogical and chemical techniques. Two types of Roman mortars were differentiated
according to this study; one contained pozzolana and the other did not contain
pozzolana [8].

    This study was aimed, firstly, at analyzing the plasters and mortars used at the
archaeological site of Barsinia, dating back to different periods, to understand the de-
velopment of the construction techniques used, chronologically. Secondly, character-
izing the compositional and textural features of the mortar and plaster, substantially
provides information on potential mortars that can be employed for conservation pur-
poses at the site.

   Mortar is a diachronic building material, used for bonding solid pieces of stone or
brick for protective or decorative coverings in floors and substrates. Mortar is produced
by mixing a binder with sand aggregates or an inorganic additive. Different types of
binders can be distinguished; these include mud, gypsum, lime, pozzolan, hydraulic




                                                                                                 CONSERVATION SCIENCE IN CULTURAL HERITAGE
lime, cement or a mixture of them [9, 10].
   However, lime binder has been the most frequently used traditional material in
the building industry for more than three thousand years. Early civilizations, such
as the Incas, Mayas, Chinese, Egyptians, ancient Greeks and Romans, used lime
as a binder in brick or stone masonry structures and for rendering masonry sur-
faces [11].

   In Jordan, lime plasters and mortars were used even earlier; examples of such
materials have been found at Ain Ghazal archaeological site and have been dated
to the Neolithic Period (ca. 7000 BCE). The people of Ain Ghazal used lime mortar
and plaster as materials for both construction and decoration. The famous statues
of Ain Ghazal were made using this type of material [12, 13].




                                                                                            65
M. Mohammad AL-Naddaf, L. Salem EL-Khouri - Mineralogical and textural characterization of mortars and plasters




                                                                                                                           Figure 3. A piece of plaster in Area A, Square B10 (sample Br.06.A.B10.05)




                                                                                                                     2. Materials and Methods

                                                                                                                     2.1. Samples

                                                                                                                     The study sampled 12 plaster and mortar pieces dating from early Hellenistic to
                                                                                                                  Umayyad periods and come from 12 different structures at Barsinia. The studied sam-
                                                                                                                  ples represent the only samples that were collected from the site during two seasons of
                                                                                                                  excavations. The first was conducted in 2006, when 11 samples out of the total number
                                                                                                                  of samples were excavated, while during the last excavation season in 2007, only
                                                                                                                  sample number Br.07.B.A3 was uncovered. The volume of the excavated samples
                                                                                                                  ranges from about 15 cm3 (ca. 5cm x 3cm x 1cm) to about 1300 cm3 (20 cm x13cm
                                                                                                                  x 5 cm). The samples were dated according to the associated archaeological objects
                                                                                                                  and the chronological sequence at the site (Table 1).

                                                                                                                     2.2. Petrographic Investigations

                                                                                                                      Because some of the studied samples were fragile, preparation of the thin sections
                                                                                                                  for petrographic examination required pre-consolidation; therefore, the samples were
                                                                                                                  impregnated with Epoxy resin under vacuum. Thin sections were prepared as suggest-
                                                                                                                  ed by Lewis and McConchie (1994) [14], but instead of using water as a lubricant, oil
                                                                                                                  was used to avoid damaging the water soluble minerals [15]. To differentiate between
                                                                                                                  the carbonate minerals in the samples, the thin sections were dyed with a solution
                                                                                                                  containing alizarin red-S in 2% hydrochloric acid (HCl) [14,16]. This solution is normally
                                                                                                                  used by sedimentologists to differentiate between calcite and dolomite. In this study,
                                                                                                                  it was used to distinguish between lime binder and calcite aggregate, based on the
                                                                                                                  fact that lime binder has fine-grained crystals - and consequently a large surface area


                                                                                                             66
- that etch more rapidly and show a more intense colour than coarser crystals (calcite
aggregates). As a result, the contrast between the binder and the aggregate can be
enhanced [17], making determination of the binder/aggregate ratio more accurate.

   A Leica polarizing microscope was used to petrographically examine the prepared
thin sections. One of the most important properties that determine the durability and
specifications of a lime mortar is the weight proportion of aggregate/binder; therefore,
lime mortar analysis for conservation purposes commonly involves the quantification
of binder/aggregate ratio by weight. The mix proportion of the studied mortar was cal-
culated by using a Prior J0415G point-counter; at least 300 counts were made for each
sample according to procedures described by the International Union of Laboratories
and Experts in Construction Materials, Systems and Structures (RILEM) TC-COM C2.
Referring to this procedure, the weight proportion of aggregate/binder (F) is calculated
using the equation:




   where




                                                                                                  CONSERVATION SCIENCE IN CULTURAL HERITAGE
   Density of aggregate is approximately 2.67 g/cm3, density of the lime paste is about
1.2 g/cm3, mole weight of CaCO3 is 100, and mole weight of Ca(OH)2 is 74.




  The portion coarser than 63 µm, which represents aggregate, was extracted by
gentle crushing and wet sieving after treatment with diluted HCl to get rid of any re-
mains of calcium carbonate binder.

   2.3. X-Ray diffraction

   Mineralogical characterization of the mortar was obtained by XRD analyses, using a Shi-
madzu Lab X, XRD-6000 X- Ray Diffractometer. Powder diffraction patterns were obtained
by applying the following conditions: CuK∝ (Copper K Alpha) radiation (1.5418 Å) with 30
kV, 30 mA energy and Graphite Monochromator. The characterization of historical mortars
by XRD was performed on the whole sample, and on the finer fraction (<63 µm).


                                                                                             67
                                                                                                                     2.4. Carbonate content

                                                                                                                     Carbonate content in the studied samples was determined using the “Dietrich-Fruhling
                                                                                                                  gas volumetric method” calcimeter that meets standards DIN 19684. The method is based
                                                                                                                  on measurement of the CO2 volume developed by the HCl reacting with the powdered
                                                                                                                  rock. The total carbonate is obtained using a formula that takes into account the pressure,
M. Mohammad AL-Naddaf, L. Salem EL-Khouri - Mineralogical and textural characterization of mortars and plasters




                                                                                                                  temperature, amount of the previously weighed sample, and the volume of CO2 developed
                                                                                                                  by the sample. In this study 300 mg of powdered bulk sample was dissolved using 1 N
                                                                                                                  HCl and the amount of CO2 released from the sample was measured using a Dietrich-
                                                                                                                  Frühling™ calcimeter. The amount of CO2 released from the samples was then compared
                                                                                                                  with that released from the same mass of a standard pure calcium carbonate sample.

                                                                                                                  Table 1. Description of the studied mortar and plaster samples

                                                                                                                   Registration No.        Source of sample              Date            Sample description
                                                                                                                   Br.06.A.A1.11           Plaster                 Late    Byzantine     Soft, yellowish, made of
                                                                                                                                                                   (5th century AD).     one layer, unpainted, fine-
                                                                                                                                                                                         grained, less than 7 mm
                                                                                                                                                                                         thick, contains organic
                                                                                                                                                                                         remains.
                                                                                                                   Br.06.A.A1.08           Bedding mortar          Late Roman (3rd       Hard, yellowish, made
                                                                                                                                                                   – 4th century AD).    of two layers, the outer
                                                                                                                                                                                         layer is light brown with
                                                                                                                                                                                         chert and organic remains,
                                                                                                                                                                                         medium-grained,        with
                                                                                                                                                                                         a thickness of about
                                                                                                                                                                                         8-11 mm. The inner part
                                                                                                                                                                                         contains chert and organic
                                                                                                                                                                                         remains,     softer   than
                                                                                                                                                                                         the outer zone, coarse-
                                                                                                                                                                                         grained, with a thickness
                                                                                                                                                                                         of more than 15mm.
                                                                                                                   Br.06.A.B10.05          Plaster                 Late Byzantine -      Soft, made of two layers,
                                                                                                                                                                   Umayyad               the outer layer is painted
                                                                                                                                                                   (6th – 8th century)   with a light brown color and
                                                                                                                                                                                         has a thickness ranging
                                                                                                                                                                                         between 1 and 3 mm. The
                                                                                                                                                                                         inner zone is light colored,
                                                                                                                                                                                         charcoal was detected in
                                                                                                                                                                                         both layers, the sample
                                                                                                                                                                                         has a total thickness of
                                                                                                                                                                                         about 3 cm.
                                                                                                                   Br.06.NecI.Tomb1.1      Bedding mortar          Late Roman –          Soft, made of two layers,
                                                                                                                                                                   Byzantine (3rd –      the outer zone is fine-
                                                                                                                                                                   5th century AD).      grained and light brown in
                                                                                                                                                                                         color, it contains organic
                                                                                                                                                                                         remains, with a thickness
                                                                                                                                                                                         of about 5 mm. The inner
                                                                                                                                                                                         zone is white colored and
                                                                                                                                                                                         coarse-grained with a
                                                                                                                                                                                         thickness of about 8 mm.
                                                                                                                   Br.06.A.C1.16           Floor mortar            Hellenistic           A compact floor, hard,
                                                                                                                                                                   (2nd century BC).     white to yellow, more
                                                                                                                                                                                         than 5 cm thick, made of
                                                                                                                                                                                         one layer. Very coarse-
                                                                                                                                                                                         grained, some grains are
                                                                                                                                                                                         about 1 cm in size.



                                                                                                             68
Br.06.A.A9.7a    Plaster          Late Hellenistic - early Plaster on a cistern
                                  Roman (1st century wall, hard to soft,
                                  BC - 1st century AD). consists of two parts,
                                                           the outer layer has
                                                           a thickness of about
                                                           7 mm, dark brown
                                                           to black in color and
                                                           contains       coarse
                                                           aggregates, the inner
                                                           part is the underlying
                                                           soil, it has a black
                                                           color and contains
                                                           charcoal. The sample
                                                           contains chert grains.
Br.06.A.A1.04    Plaster          Late Byzantine – Soft, grey, made of
                                  Umayyad (6th – 8th one layer, contains
                                  century AD).       organic remains, it
                                                     has a thickness of
                                                     more than 9 mm.
Br.07.B.A3.5     Plaster          Late Byzantine – Soft, yellowish, made
                                  Umayyad             of one layer, medium-
                                  (6th – 8th century) grained,      contains
                                                      organic remains.
Br.06.A.A1.11b   Plaster          Byzantine                  Soft, yellowish, made
                                  (5th century AD).          of one layer, unpainted,
                                                             fine- grained, less than
                                                             7mm thick, contains
                                                             organic remains.
Br.06.A.A1.c     Plaster          Late Byzantine        – Soft    to   medium,
                                  Umayyad                 made of 2 layers, the
                                  (6th - 8th century)     outer zone is white
                                                          to yellow and has
                                                          a thickness of less
                                                          than 1 mm, the inner




                                                                                             CONSERVATION SCIENCE IN CULTURAL HERITAGE
                                                          part is darker and
                                                          thicker, and is more
                                                          than 8 mm thick.
                                                          The sample contains
                                                          organic remains.
Br.06.A.C1.15    Bedding mortar   Roman                      Mosaic mortar, soft,
                                  (3rd – 4th century         white colored, very
                                  AD).                       fine-grained,   more
                                                             than 6 mm thick.
Br.06.A.A9.7b    Plaster          Late Hellenistic – Early   Plaster on a cistern
                                  Roman (1st century         wall, hard to soft,
                                  BC.– 1st century AD).      made of 2 layers. The
                                                             outer layer is tough
                                                             and is light brown
                                                             with   dark    spots,
                                                             contains chert, 5-6
                                                             mm thick. The inner
                                                             zone is black and
                                                             contains chert and
                                                             organic remains.




                                                                                        69
                                                                                                                  Carbonate content was then calculated by applying the following equation:
M. Mohammad AL-Naddaf, L. Salem EL-Khouri - Mineralogical and textural characterization of mortars and plasters




                                                                                                                  Three measurements were conducted for each sample and the average was calculated.




                                                                                                                     2.5. Physical properties

                                                                                                                     The porosity and density of the study samples were measured according to proce-
                                                                                                                  dures recommended by RILEM (1980); tests No. I.1 and I.2 as follows:
                                                                                                                     After drying to a constant mass, the samples were put in an evacuation vessel and
                                                                                                                  the pressure was gradually lowered. A constant low pressure was maintained for 24
                                                                                                                  hours. Distilled water was then slowly introduced into the vessel until the samples were
                                                                                                                  completely immersed. The samples were left for 24 hours underwater at atmospheric
                                                                                                                  pressure. They were then weighed separately in water (hydrostatic weight). The sam-
                                                                                                                  ples were quickly wiped with a dampened cloth and weighed in the air. The following




                                                                                                                  formulas were applied to calculate the density and porosity:



                                                                                                                     σabs: absolute density in g/cm3
                                                                                                                     σapp: apparent density in g/cm3
                                                                                                                     ρ: porosity
                                                                                                                     M1: dry mass
                                                                                                                     M2: mass taken under water (hydrostatic weight)
                                                                                                                     M3: wet mass in air [18].

                                                                                                             70
  3. Results and discussion

   According to the calcimetry results (Table 2), the carbonate content in all of the
samples, except sample Br.06.A.C1.16, was high. It ranged between 4% and 89%.
The average carbonate content was 65.6%. The portions finer than 63 μm contained
more carbonate compared to the whole sample. The carbonate content in this portion
ranged between 9.0 - 91.1% averaging 74.7%.


                         Table 2. Composition of the studied samples


                      CaCO3 content (%)                             XRD results

                                                  Complete sample             Grain size < 0.063 mm


  Registration No.     In the     In the    Calcite    Quarzo   Apatite   Calcite     Quarzo   Apatite
                     complete   portion <
                      sample     63 μm

  Br.06.A.A1.11        70.1       80.6      ***        **       *         ***         **       -


  Br.06.A.A1.08        63.3       77.0      ***        **       *         ***         **       -

 Br.06.A.B10.05        70.9       73.5      ***        **       -         ***         **       -

   Br.06.NecI.         68.3       69.7      ***        **       *         ***         **       -
    Tomb1.1
  Br.06.A.C1.16        4.1         9.0      *          ***      -         *           ***      -

  Br.06.A.A9.7a        61.1       79.1      ***        **       -         ***         **       -




                                                                                                              CONSERVATION SCIENCE IN CULTURAL HERITAGE
  Br.06.A.A1.04        70.1       86.0      ***        **       *         ***         **       -

  Br.07.B.A3.5         81.9       83.9      ***        **       *         ***         **       -

 Br.06.A.A1.11b        75.4       85.6      ***        **       *         ***         **       -

  Br.06.A.A1.c         66.6       81.3      ***        **       *         ***         **       -

  Br.06.A.C1.15        89.0       91.1      ***        **       *         ***         **       -

  Br.06.A.A9.7b        62.2       78.7      ***        **       -         ***         **       -




                                                                                                         71
                                                                                                                      The qualitative results of the XRD analysis are presented in Table 2 and Figure 4. Ex-
                                                                                                                  cluding sample Br.06.A.C1.16, calcite showed no significant quantitative differences in its
                                                                                                                  content, in the mortars examined. All of the samples, except for sample Br.06.A.C1.16,
                                                                                                                  were made of calcite (CaCO3) which was the main constituent and quartz (SiO2) in a
                                                                                                                  lower proportion. Sample Br.06.A.C1.16 is mainly made of quartz and contains a smaller
                                                                                                                  amount of calcite. Traces of the mineral, Apatite, were detected in most of the samples; its
M. Mohammad AL-Naddaf, L. Salem EL-Khouri - Mineralogical and textural characterization of mortars and plasters




                                                                                                                  presence can be attributed to the addition of animal bones to the mortars and plasters of
                                                                                                                  Barsinia. The addition of bone ash to the plaster facilitates the process of plastering by in-
                                                                                                                  creasing the plasticity of the mortar. Furthermore, the presence of bone in mortar and plas-
                                                                                                                  ter decreases the possibility of cracking and consequently increases their durability [19].




                                                                                                                            Figure 4. Powder X-ray diffraction pattern for 3 representative mortar
                                                                                                                            samples. Qz. is quartz, Ca. is calcite and Ap. is apatite




                                                                                                                     For the grain size finer than 63µm, which is mainly made of a binding material, XRD
                                                                                                                  results showed that the relative abundance of calcite and quartz in this portion is the
                                                                                                                  same as in the whole sample. The only difference between the mineralogical composi-
                                                                                                                  tions of this portion with that of the whole sample is the absence of apatite in the grain
                                                                                                                  size finer than 63µm in the samples. No calcium silicate mineral could be detected in
                                                                                                                  any of the studied mortars; a result which indicates a non-hydraulic mortar or which
                                                                                                                  may be attributed to the fact that the structures of calcium silicate produced by poz-
                                                                                                                  zolanic reactions are somewhat difficult to analyze, because calcium silicates are very
                                                                                                                  fine and are not easily distinguished with XRD or by microscope [6].



                                                                                                             72
    In addition to the minerals detected by XRD, other components were identified by
using stereo and polarizing microscopes. Table 3 shows the modal analysis results ob-
tained by using a stereo microscope for grain size coarser than 63µm, which is made
of aggregate and contains no binding material. The results showed that the composition
of the grains coarser than 63µm varies considerably in the studied mortars; calcite and/
or quartz are the major components in many of the studied samples. The aggregate in
some samples is mainly made of pottery fragments. Four of the samples revealed a con-
siderable amount of chert, and volcanic ash was found in 3 others. Occasional fragments
of charcoal were identified in 2 samples; their sporadic presence suggests that they are
accidental, probably due to contamination from the kiln fuel. Most of the samples con-
tained remains of organic materials (Fig. 5, Table 3). Although the studied samples are
dated to different historical periods, the petrographic investigation showed that they have
homogenous, cohesive binders displaying a strong aggregate-binder bond, in all of them
the lime binders are fine-grained, rarely displaying shrinkage cracks (Fig. 5).
    Some of the studied samples contained underburned lime particles (Fig. 5a). Evi-
dence of binder-aggregate reaction was found in several mortars and the presence of
ceramic fragments, chert, volcanic ash and /or fuel remains, acting as pozzolans, was
also recorded in some samples (Figs 5b and 5c).
    According to Pavìa (2005), the absence of binder cracks indicates a low shrinkage
of the mortar binding materials. The high specific surface of the lime and low shrinkage
suggest that the raw limestone was soft-burned [15].


     Table 3. Modal analysis results of the aggregate as shown by the stereo microscope

   Registration         Quartz   Calcite   Pottery    Chert     Volcanic    Organic
   No.                                     fragment             ash         material
                                                                            remains




                                                                                                   CONSERVATION SCIENCE IN CULTURAL HERITAGE
   Br.06.A.A1.11        60       25        10         5         0           2
   Br.06.A.A1.08        7        15        0          60        10          8*
   Br.06.A.B10.05       35       5         25         35        0           0
   Br.06.NecI.          15       30        50         0         0           5*
   Tomb1.1
   Br.06.A.C1.16        6        4         0          90        0           0
   Br.06.A.A9.7a        15       6         5          74        0           0
   Br.06.A.A1.04        20       10        60         5         5           1
   Br.07.B.A3.5         15       30        55         0         0           2
   Br.06.A.A1.11b       55       40        5          0         0           1
   Br.06.A.A1.c         54       40        5          0         <1          1
   Br.06.A.C1.15        35       65        0          0         0           2
   Br.06.A.A9.7b        20       5         10         65        0           0

  *: mainly charcoal.




                                                                                              73
                                                                                                                      Boynton (1966) and Cowper (2000) reported that low burning temperatures and/
                                                                                                                  or shorter burning duration produce a desirable soft-burned quicklime, which is highly
                                                                                                                  reactive and of low shrinkage and density and high porosity, whereas a high burning
                                                                                                                  temperature and long calcining periods result in a hard-burned quicklime that has high
                                                                                                                  shrinkage, high density, low porosity and low chemical reactivity [20, 21]. The higher
                                                                                                                  reactivity of the binder in some of the studied mortars is evidenced by the occurrence
M. Mohammad AL-Naddaf, L. Salem EL-Khouri - Mineralogical and textural characterization of mortars and plasters




                                                                                                                  of the reaction rims around grains having pozzolanic effects, such as chert (Fig. 5b).

                                                                                                                      Excluding sample Br.06.A.C1.15, which is a mosaic mortar, all of the studied mor-
                                                                                                                  tars are more or less hydraulic; they contain one or more type of pozzolanic material,
                                                                                                                  i.e. pottery fragment, chert, volcanic ash and/or charcoal. However, according to pet-
                                                                                                                  rographic analysis, most of the mortars were made with non-hydraulic lime and their
                                                                                                                  hydraulicity is due to the addition of materials acting as pozzolans. This agrees with
                                                                                                                  the findings of Vicat (1997), who reported that the first production of calcined hydraulic
                                                                                                                  lime was around the second half of the 18th century, i. e. much later than the studied
                                                                                                                  mortar [22].
                                                                                                                      The weight proportion of aggregate/binder (F) in the archaeological mortars of Bars-
                                                                                                                  inia is shown in Table 4. Only 4 samples had an (F) higher than 1; these are samples
                                                                                                                  (Br.06.A.C1.16, Br.06.A.A1.08, Br.06.A.A9.7a and Br.06.A.A9.7b). Three of these sam-
                                                                                                                  ples were dated to the Hellenistic period, with a high content of pozzolanic materials.
                                                                                                                  The other samples had a value of less than 1, indicating that most of the mortars in
                                                                                                                  Barsinia contain a relatively higher binder content.

                                                                                                                      Many studies of historic mortars have generated results suggesting compositions
                                                                                                                  with an (F) of 1, i.e. 1 part lime binder: 1 part aggregate, in contrast to the 1: 3 (F = 3)
                                                                                                                  ratio commonly specified in current building work [23]. Sample Br.06.A.C1.16 has a
                                                                                                                  very high (F); this sample, which is a compact floor, contains a high content of coarse
                                                                                                                  aggregates. Three other samples have an (F) close to 3; they resemble the mix pro-
                                                                                                                  portion in present-day mortar. The high binder content in the other samples, samples
                                                                                                                  with a low (F), could be attributed to the presence of unmixed binder, fragments of
                                                                                                                  lime lumps that have not been fully mixed with the aggregate, and consequently have
                                                                                                                  physical and chemical properties that differ from the matrix paste. As they do not play
                                                                                                                  the role of a binder during the hardening process, the studied mortars (even those with
                                                                                                                  high binder content) do not show any notable cracking, in spite of the fact that a high
                                                                                                                  binder content in mortars tends to cause cracking.
                                                                                                                      The aggregate/binder ratio per weight in flooring mortars is much higher than that in
                                                                                                                  lining mortars and plasters. The plasters taken from cisterns (samples Br.06.A.A9.7a
                                                                                                                  and Br.06.A.A9.7b) contained relatively higher aggregate content in which a consid-
                                                                                                                  erable concentration of pozzolanic components could be detected. The presence of
                                                                                                                  such components in the plaster gives the mortar and plaster their hydraulicity, less
                                                                                                                  solubility in water and more stability. The relatively high content of pozzolanic materi-
                                                                                                                  als in these samples is consistent with the historical fact that pozzolanic components
                                                                                                                  were preferred during Hellenistic and early Byzantine times for use in mortars related
                                                                                                                  to water-bearing constructions such as cisterns [24, 25]. The porosity of this type of
                                                                                                                  plaster is relatively less than that of other plasters and mortars.




                                                                                                             74
            Table 4. Weight proportion of aggregate/binder for the studied mortars


    Registration No.           Points
                                                 Weight proportion of aggregate/binder (F)
                          Paste         Aggre
                                         gate
     Br.06.A.A1.11                314                    72                     0.68
     Br.06.A.A1.08                146                   181                     3.54
    Br.06.A.B10.05                247                    63                     0.31
  Br.06.NecI.Tomb1.1              345                    28                     0.24
     Br.06.A.C1.16                 8                    312                    150.7
     Br.06.A.A9.7a                189                   173                     2.73
     Br.06.A.A1.04                242                    61                     0.28
     Br.07.B.A3.5                 321                    47                     0.43
    Br.06.A.A1.11b                356                    43                     0.31
     Br.06.A.A1.c                 367                    58                     0.45
     Br.06.A.C1.15                517                    46                     0.22
     Br.06.A.A9.7b                183                   175                     2.86


    Table 5 shows the physical properties of the studied samples. The relatively low dif-
ference between the water uptake under atmospheric pressure and the water uptake
under vacuum in all of the studied mortars is attributed to the low portion of micropores;
in fact, most of the studied mortars have a saturation degree above 0.85. The results
from the porosity tests showed that the porosities of the samples are higher than those




                                                                                                    CONSERVATION SCIENCE IN CULTURAL HERITAGE
in the typical range of historical lime mortars [15]. The porosity of the samples varied
between 32.78 and 68.35%. Based on these results the samples can be classified into
2 groups. The first group comprising samples with porosities of less than 45% (sam-
ples Br.06.A.C1.16, Br.06.A.A1.08, Br.06.A.A9.7a and Br.06.A.A9.7b) are the samples
with the highest apparent densities (1.46 and 1.78 g/cm³). The second group repre-
sents the samples with porosities higher than 50% and low densities (0.81-1.30 g/cm³);
these samples have low weight proportions of aggregate/binder (F) ranging between
0.22 - 0.68. Porosity of mortars and plasters plays two different roles as regards their
durability. On the one hand, a good porosity allows an extra interchange surface as-
similating carbon dioxide, which will enhance the carbonation process of the slaked
lime to produce calcium carbonate [26]. On the other hand, mortars and stones with a
high porosity are more susceptible to deterioration under the effect of frost, salt crystal-
lization and chemical deterioration factors. According to Sanchez-Moral et al. (2005)
the high porosity of mortars and plaster can be attributed to cracking after drying linked
to the high binder content [26]. However, most of the samples did not show such crack-
ing. Instead, most of the samples contain remains of organic materials, such as straw
and bones; the decomposition of these materials leaves cavities which increases the
porosity of the mortars and plasters.




                                                                                               75
                                                                                                                                           Table 5. Physical properties of the studied samples


                                                                                                                   Sample No       Water            Water         Porosity     Saturation    Absolute   Apparent
                                                                                                                                   uptake under     uptake                     degree        density    density
                                                                                                                                   atmospheric      under
                                                                                                                                   pressure         vacuum
M. Mohammad AL-Naddaf, L. Salem EL-Khouri - Mineralogical and textural characterization of mortars and plasters




                                                                                                                                   Mass %           Mass%         Vol.%        /             g/cm³      g/cm³
                                                                                                                  Br.06.A.A1.11    41.38            46.27         55.27        0.89          2.67       1.19
                                                                                                                  Br.06.A.A1.08    18.81            22.20         37.25        0.86          2.67       1.68
                                                                                                                  Br.06.A.B10.05   59.04            64.14         62.15        0.92          2.56       0.97
                                                                                                                   Br.06.NecI.     76.57            84.06         68.35        0.91          2.57       0.81
                                                                                                                    Tomb1.1
                                                                                                                  Br.06.A.C1.16    16.03            18.40         32.78        0.87          2.65       1.78
                                                                                                                  Br.06.A.A9.7a    18.83            20.43         34.61        0.92          2.59       1.69
                                                                                                                  Br.06.A.A1.04    46.96            50.72         56.79        0.93          2.59       1.12
                                                                                                                   Br.07.B.A3.5    40.03            47.24         55.95        0.85          2.69       1.18
                                                                                                                  Br.06.A.A1.11b   40.11            45.32         54.86        0.88          2.68       1.21
                                                                                                                   Br.06.A.A1.c    43.08            47.36         55.27        0.91          2.61       1.17
                                                                                                                  Br.06.A.C1.15    28.00            30.02         43.91        0.93          2.61       1.46
                                                                                                                  Br.06.A.A9.7b    34.30            39.49         51.40        0.87          2.68       1.30



                                                                                                                      4. Conclusions

                                                                                                                      Although only a limited number of samples was available for this study, the phys-
                                                                                                                   icochemical characterization of the samples from the archaeological site of Barsinia
                                                                                                                   revealed significant compositional and textural differences. Consequently, no general
                                                                                                                   restoration mortar or plaster can be adopted for the whole site to replace the original
                                                                                                                   deteriorated one.

                                                                                                                      The high porosity of the mortars and plasters seems to be the most important intrin-
                                                                                                                   sic deterioration factor causing their deterioration. The saturation degree of the studied
                                                                                                                   samples is higher than 0.85; stones and mortars having such a value are highly sus-
                                                                                                                   ceptible to frost damage [27, 28]. Therefore, to protect them, mortars and particularly
                                                                                                                   plasters, should be consolidated with an appropriate consolidant immediately after
                                                                                                                   being excavated.

                                                                                                                       The compositional and textural differences among the samples seem to be linked
                                                                                                                   to the function of the mortars rather than their time of production, i. e. no evolution
                                                                                                                   on the techniques to produce the mortar at the site could be traced. The XRD results
                                                                                                                   showed that no important differences in the mineralogical composition could be de-
                                                                                                                   tected among the studied mortar and plaster, except in sample Br.06.A.C1.16; all the
                                                                                                                   samples were mainly made of calcite and quartz, minerals which are locally available
                                                                                                                   in the limestone rocks and sediments at the site. However, the petrographic investiga-


                                                                                                             76
tions revealed considerable compositional differences among the samples in terms of
intentionally added components such as bone ash, pozzolanic materials, etc.

   The high porosity, strong binder cohesion and perfect aggregate-binder bond of
most of the analyzed mortars, together with the presence of aggregate-binder reaction
denotes a high reactivity for the lime, that also agrees with soft burning which produces
the best lime mortar. Accordingly, the people of Barsinia had the necessary knowledge
and experience to manufacture mortars and plasters of a good quality.

   Thanks to the physicochemical characterization conducted in this study, it is possi-
ble to prepare a restoration mixture having characteristics compatible with the original
mortars and stone in the masonry structure to be used for the restoration of the struc-
tures in Barsinia and other similar archaeological sites.




                                                                                                 CONSERVATION SCIENCE IN CULTURAL HERITAGE
               Figure 5. Photomicrograph (X100): a. XPL showing underburned
               lime, b. XPL showing reaction rim around chert grain and c. PPL
               charcoal



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     Berlin, pp. 563-571.


  Biographical notes

   Mustafa Al-Naddaf is Associate Professor at the Dept. of Conservation and Man-
agement of Cultural Resources and Vice Dean of the Faculty of Archaeology and An-
thropology, Yarmouk University in Jordan. He holds a B.Sc., M.Sc. in geology and
Ph.D. in stone conservation from the Free University of Berlin, and Rathgen-Forschun-
gs Labor, Germany. His research interest generally concentrates on areas of conser-




                                                                                                 CONSERVATION SCIENCE IN CULTURAL HERITAGE
vation and the scientific analysis of archaeological materials.

    Lamia El-Khouri is Associate Professor at the Dept. of Archaeology, Yarmouk Uni-
versity in Jordan. She holds a B.A., M.A., in Archaeology, and a Ph.D., in Classical
Archaeology from Manheim University, Germany. Her research interest focuses on
different topics in Classical Archaeology in the East.




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