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J. Asiat. Soc. Bangladesh, Sci.

38(2): 145-153, December 2012

ELEMENTAL ANALYSIS OF OLD MORTAR USED IN VARIOUS
ARCHAEOLOGICAL SITES OF BANGLADESH BY SEM AND EDAX
ACHIA KHANOM1,*D. K. SAHA2, S. M. RAHAMAN1 AND AL MAMUN2
1
Department of Archaeology, Jahangirnagar University, Savar, Dhaka
2
Materials Science Division, Atomic Energy Centre, Dhaka-1000

Abstract
Morphological characterization and mineralogical studies were performed on fifteen
mortar samples collected from three ancient archaeological sites (Wari-Bateshwar,
Lalmai-Mainamati, and Paharpur) of Bangladesh. Many cracks and pores were found in
the mortar samples of Buddhist Lotus temple of Wari-Bateshwar. Energy dispersive
analytical x-ray analysis confirmed the presence of C, O, P, K, Al, Fe, Na, Mg, Mn, Si
and Ti in the mortar samples. The absence of Ca in the samples indicates that the clay
was used in the architecture as binding materials. In the clay mortar, Si played an
important role and with the presence of O2, SiO2 was formed, which strengthened the
binder. K, Al, Fe, Na, Mg, Mn, Si and Ti might form compounds like SiO2, Fe2O3, K2O,
Al2O3, MgO, MnO, Na2O3, and TiO2 with O2. The oxidation of Fe+2 produced Fe2O3
which was responsible for breaking down the bonding of mortars.
Key words: Archaeology, Mortar, Deterioration, SEM and EDAX

Introduction
Mortar analysis is an essential domain for conservation of architectural remains of
Bangladesh. Mortar, a workable paste, generally formed by the mixture of cement, sand
and water, is a fine aggregate to fill the gaps between construction bricks and stones.
Aziz (1995) classified the types of mortar as follows (i) mud mortar (ii) lime mortar (iii)
surki mortar (iv) lime surki mortar and (v) cement mortar. In the world context, the mud
mortar was made from the mud clay. In early Egyptian time (2600-2500 B.C.), pyramids
were constructed using limestone blocks that were bound either by mud and clay or clay
and sand mortar. Later on, a different mortar was used for constructing Egyptian pyramid
which was made of either gypsum or lime. The lime mortar was used in ancient Egypt
before 4000 B.C. (Wikipedia 01-07-2012). Different types of mortar have been used in
masonry building construction since ancient to date in Bangladesh. Present research is to
focus on elemental analysis of old mortar used in various archaeological sites (WariBateshwar, Lalmai-Mainamati, and Paharpur) of Bangladesh.
Brief history of the study sites
Wari-Bateshwar (5th Century B.C.): Wari-Bateshwar is an important early historic
archaeological site of Bangladesh located at Belabo Upazila in Narsingdi. The two
1

Corresponding author: Email: likhon000@yahoo.com

Charpatra Mura. .D. Paharpur main temple at Naogaon. a small cruciform temple (Photo 2) and stupa near to Salban Vihara were discovered. it is assumed that Wari-Bateshwar was the ancient trade centre named ‘Sounagara’ as mentioned by the Greek geographer Ptolemy (Rahman 2001). large number of stupa and monastery indicate that the site was flourished from 7th to 13th centuries A. Itakhola Mura. Small cruciform temple at Vihara. These are Salban Vihara. Ali and Alam (2000) and Rashid (1997) reported that some structural remains have been discovered by excavation at Lalmai-Mainamati from 1955 to 2000. were built. Rupban Mura. Lati coat Mura. Rashid (1997) reported that it was the second largest city of ancient Bangladesh in which the religious establishment. Lalmai-Mainamati (6th to 13th centuries A. During excavation (2000-2009). In recent research. During (2008-2009) excavation. thousand five hundred years old fort-city stands on the bank of the river Brahamhaputra. a unique brick architecture with dimension 18 m × 32 m was discovered (Photo 1). Unique brick architecture at WariBateshwar.146 Khanom et al. Among the 48 archaeological sites discovered in Wari-Bateshwar region. Anada Vihara. and Queen Mainamtai’s palace mound.D.): Lalmai-Mainamati was one of the attractive places for the Buddhist community. Kutila Mura. Wari is configured as the nucleus of the sites. Hossain (2007). Photo 1. together with large Viharas and the constituent’s colleges of the Buddhist University. Bhoja Vihara. Salban Photo 3. Photo 2. Ahmed (1975) and Rashid (1997) reported that huge collection of artifacts.

. specification of mortars and characteristics of various lime mortars. Akasheh et al. square. (2008) have analyzed mortar from southern Portugal cathedrals (Evora e Elvas) by optical microscopy and XRD. . and votive stupas are the main features of Paharpur archaeological site. Brocken et al. TGA (Thermogravimethic Analysis). 2003 and 2009) reported in his book ‘Archaeomineralogy’about the aggregate used in ancient mortar. Ca. with the help of UNESCO. Fe. viz. micro crystal structure. SEM (Scanning Electron Microscopy). Alam (2004) reported that. Válek (1995). Rapp (2002. 1930-32 and Dikshit in 1928-29 and 1934 under the supervision of Archaeological Survey of India (ASI).): The archaeological remains of Paharpur (World Cultural Heritage Site) represent the most spectacular and magnificent monument of Bangladesh. 2008). Most of the modern European researchers like Bentz and Momber (2002 and 2003). mass and aging of mortars.D. chemical analysis. Jordan et al. chemical analysis and 14C dating. Literature Review: Mortar analysis is a multidisciplinary task (Patricia et al. Rectangular monastery with 177 cells and Varanda. They found that quartz. NMR (Nuclear Magnetic Resonance) Spectroscopy. Al. Atomic absorption Spectroscopy. The results indicate that the crushed ceramic particle was used as raw materials in the mortar. kaolinite. by using different scientific methods such as XRD (X-Ray Diffractometer). (2001). different types of stupa. octagonal. Velosa et al. process of cracks extension. (2006). IR (IR-Infra-red) Spectroscopy. feldspar. particle size. Habesch (2006) studied the biofilm (fungi and algae) distribution on mortar surfaces by SEM and EDAX. They have focused on the characterization. Ellis (2002) studied the morphological. execution and visualization of thin sections by thermal analysis. (2003-05) studied mortars from Archaeological Sites at Petra of Mediterranean area by FTIR and XRD analysis. textural and compositional interrelationships of mortar by SEM and elemental analysis by EDAX. Excavation at Paharpur was carried out by G. Mg. mica. Mass Spectroscopy. conductivity. Valckenborg et al. and Si were determined by SEM. composition. 1984-85. and Petkovic (2005) discussed mainly on the use of mortar from the 14th to 20th centuries. the Department of Archaeology skillfully excavated the site in 1981-82. It is also known as Somapura Mahavihara (Photo 3). a cruciform temple. elemental analysis. amphiboles and calcite minerals are present in the mortars. mineralogical study. They found calcite. star shape. pH.C. (2006) have studied mortars from the wall of cattle tank in Newcastle where K. 1988-89 and 1990-91 and three major building phases in the monastic cells were established. Rijniers (2004). dolomite. Patricia et al. Mortar compounds such as quartz and lime were detected. They have found SiO2 and CaCO3 in the samples by XRD analysis. It is the second largest Buddhist monastery situated at the South of the Himalayas. and reported history of lime mortars. XRF (XRay Fluorescence). Na. Chandra during 1925-26.Elemental analysis of old mortar 147 Paharpur (8th to 13th centuries A. porosity. (2007) studied various samples at archaeological site of Conímbriga and determined particle size distribution. mineralogical and chemical analysis using XRD and XRF. A report on Paharpur archaeological excavation was published by Dikshit in 1938.

Salts. CaO. High resolution FEI S50 scanning electron microscope was used. Candeias et al.ion were found in the restored mortar sample of Paharpur by chemical analyses.00%). Al2O3. pozzolanic products or organic/biological microorganisms were determined by SEM. The collected mortar samples were cleaned followed by laboratory test. illite and chlorite were determined in the soil samples. Lalmai-Mainamati. Big size pores were found (20 µm) in the samples of WBBLT-4 which indicate weakening of the joint areas. chlorite. Al2O3 (5.10%) by chemical analysis.60%). MgO and Na2O3 were determined by XRF. therefore of interest to study elemental concentration of mortar by EDAX and morphological study by SEM to determine crack and pore of mortar samples. and Paharpur to investigate the morphological characteristic and elemental concentration of mortar.90%). Pellet was cleaned by white sprit for removal of dust particles. TiO2. Materials and Methods Fifteen mortar samples were collected from the joint areas of brick masonry wall of Wari-Bateshwar. It is. Cafeldspar. Images were taken with the magnification of 100000X and the resolution of 50 to 100 nm in secondary electron scanning mode. Islam (2005) analyzed mortar from Shait Gambuz Mosque and found CaO (85. Energy dispersive X-ray method was used for elemental analysis of mortar samples. In a previous study (Khanom 2007) the terracotta plaque of Paharpur with mortar were analysed by XRD and it was found that the terracotta contains montmorillonite. P2O5.and Cl. illite. attapulgite. SiO2 (5. feldspar. EDAX was used to unveil the elemental composition of mortars. The pellets of samples were prepared in 50 mm dia. SiO2. Masud et al. Porosity and cracks were determined by optical microscope. and micrite minerals. it was observed that surface of the mortar was rough.148 Khanom et al. mainly discussed the methodology for characterization of ancient mortars from different author results. albite and calcite. quartz. Fe2O3. Surface of the pellet was polished by emary paper. SO42. specially cracks and pores of the samples. A large number of cracks were found in the samples of WBBLT 1 & 4. and 3 mm thick size for SEM and EDAX analyses. Small sizes of pores and cracks were found (1µm) in the . Fe2O3 (3. kaolinite. Solid samples were cleaned by white sprit. SEM and EDAX study: In the present study SEM was used to determine the surface morphology of the mortars. Pellet samples were fitted into the sample chamber and scan the pellets with electron beam. montmorillonite. (2008) studied mineralogy of archaeological soil of Paharpur by XRD and quartz. kaolinite. K-feldspar. MnO. quartz. SEM images were taken in secondary electron scanning mode using 25 KV accelerating voltage. K2O. Results and Discussion Morphological study of Mortar: In the present study.

which indicates strengthening of the joint areas of these sites (Fig. Na. a. b. air and ions inside the mortars. Deteriorating agents like wind. PPMT-1. flood water. Small sizes pores were found in the samples of newly discovered “Small Cruciform Temple” near the Salban Vihara at Lalmai-Mainamati. A few number of pores were found in the samples of LM-2 and PPMT-1 which indicates that the joint area is stable of these sites (Fig.1 c. which played significant role for the deterioration of mortars. ground water.Elemental analysis of old mortar 149 sample of LM-2. salt. WBUBA-1 b. Elemental analysis of mortar: Representative examples of elemental spectrum of mortar samples. atmospheric gases. Fe. acidic ion. dust and dirt. c. WBBLT-4 Crack c.1. WBUBA-1. K. P. Mn. LM-2 d. SEM images showing cracks and pores of mortar samples: a. LM-2 and d. d). Mg. It is understandable that the cracks and pores are responsible for the deterioration of mortar strength in different locations of these sites. stability of mortar was found well in Lalmai-Mainamati sites leading to less damage of the architectural remains of these sites. Hence. . 1 (a. WBBLT-4. PPMTPore Fig. where the following elements have been found: C. Al. and PPMT-1. O. These were observed in the West wall of Buddhist Lotus Temple in Wari-Bateshwar. Large number of pores and cracks are helpful for intruding rainwater. rainwater. and plant-roots can easily enter into the mortars through the pores and cracks. Pore is one of the physical criteria which enhancing deterioration of mortars as well as brick masonry walls. b).

94 wt.150 Khanom et al. 1.80 wt.98 to 35.06 to11. Less amount of Al (5. Al. Si. (c). Quartz is the most stable of all minerals in the earth surface environment (Rapp et al. Higher amount of Si and O2 might come from sand. and Ti have been determined and listed in Table 1.52 to 25. K(1. Mg.10 wt. 1930). Na. The study indicates that clay with sand has been . P. 2 individual elements are shown with their corresponding Kα and Kβ energy level.%).% of Mn has been found in the sample of WBBLT-4. O. Each element has its individual energy for its Kα and Kβ shells.6 wt. Kα and Kβ. 2. The Multi Channel Analyzer (MCA) was calibrated using known standards and then the corresponding energy level was detected for each element.12 wt.44 to 2. and Ti are presented in Fig.98 to 6. Ti and Fe show two peaks. WBUBA-1. The principal constituent was found as Si.80 wt.% have been found in most of the samples. K.%) and Mg 0.%) have been found in the mortar samples of PPMT-2 which indicate weakening the joint areas at Paharpur main temple. Higher amounts of O2 (35. Energy level (keV) Energy level (keV) Fig. K. Higher rates of O2 (21.16 wt. For each element corresponding counts was used to calculate the concentration by comparing the counts of standard of same element. Mn. Fe. EDAX spectrum showing various elements of mortar sample: (a). LM-1. Counts of all the overlapping peaks (Kα and Kβ) were separated by using Kβ / Kα ratio. LM-2 and (d). (b). Si. PPMT-1.%) have been found in all the mortar samples which might come from SiO2.%) and Si (13. Elemental concentrations of C.98 wt. In Fig. 2(a-d). Energy level of each element is shown in the parenthesis.%) and Fe (20.

06 11. K. Presence of Mg and K in the samples of Paharpur. Mg.94 14. Mn.12 Si 16.31 1.71 5.94 35.74 1.24 0.12 Fe 19.56 14.21 35.59 17. Na.94 16.99 2. Fe. Mg and K are likely to be minor constituents of the shells and or the sand (Jordan et al.25 14.05 2.86 18.26 16.21 16.27 6.97 19. Si is durable because it has high ability to preserve water and release of water easily. There might be formation of MgSO4.56 0. MgO.71 Mg 0. and Ti have been found from the EDAX analysis.98 23. The absence of CaCO3. Mg.80 29.75 13. Si.85 31.29 0.57 20.56 36.56 25. Jordan et al.70 2.65 16.17 C 24.58 0.78 24.91 18. Oxidation of Fe+2 produces Fe2O3 which was also responsible for breaking down of bonding of mortars.45 1.99 5.12 2.56 1. P.04 Na 0. Mn. Al2(SO4)3.96 15. MnO.56 0. Ca and CO3 in the samples at Wari-Bateshwar.31 0.55 30.94 20. The presence of Si in the samples of WBUBA-1-3. Si played significant role as strong element.62 29. Among these compounds SiO2 played significant role for longevity of brick masonry.66 2.75 26.23 29.51 0. Good quality of clay was used for mortar in the ancient period.46 1.12 31.98 2.72 Ti 1. and Wari-Bateshwar suggest that clay with sand were used as mortar component.31 35.98 3.05 16.44 0.16 22. Na2O3. Sample ID WBUBA-1 WBUBA-2 WBUBA-3 WBBLT-4 WBBLT-5 LM-1 LM-2 LM-3 LM-4 LM-5 PPMT-1 PPMT-2 PPMT-3 PPMT-4 PPMT-5 Al 6.54 5. KCl.28 6.76 6.77 2. Fe2O3.16 27. NaCl.50 15. LM-1 to LM-5.51 - O 27.54 0.72 29.44 0.16 K 2. All these indicate that lime mortar was used as binding materials in the architecture of this site as well as medieval architecture of Shait Gambuz Mosque and the Residence of Khan Jahan. Na.44 4. and TiO2 compounds with O2. which are responsible for breaking down the mortars (Khanom 2012).61 5. Al.87 14. WBBLT-4-5. Si and Ti might formed SiO2. O.38 6.16 4.33 16.44 3. 2006).12 2. SO42.and Clhave been found from the wet chemical analysis and Ca. and PPMT-1 to PPMT-5.06 25.66 0.51 6.09 15.40 2.89 27.83 25.10 7.74 6. and PPMT-1 to PPMT-5 indicate that clay with sand was used as mortar component for the architecture.53 28.78 30.60 1. indicates that silicate played significant role for the architecture of these sites.42 35. WBBLT-4-5. CaCO3 has been found by XRD analysis. K2O.89 26.04 1.74 15. elements like Na and Fe can assist retention of moisture and water easily and can deteriorate mortar faster than Si.76 36. CaSO4 salt.99 17.56 15.93 28. Fe. %. Table1. K. Al. Elemental concentration of mortar samples in wt. FeSO4.71 28.56 0.21 2. Presence of Al and Fe in the samples of WBUBA-1-3.66 24. Lalmai-Mainamati and Paharpur .98 5.78 28. LM-1 to LM-5.39 - On the other hand. Al2O3.34 25. (2006) reported that Al and Fe would come from the clay content of the mixing sand.09 16.Elemental analysis of old mortar 151 used as mortar.09 5.47 2.98 6.40 2.52 23.

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