CHARACTERISATION OF ANCIENT MORTAR AND SIMULATION OF

NEW MORTAR AT NAGANATHASWAMY TEMPLE, KUMBAKONAM

AND THANJAVUR PALACE FOR RESTORATION

Submitted to

The Member Secretary

State Planning Commission

Ezhilagam, Chepauk

Chennai – 600005

By

Dr. S.K. SEKAR

Senior Professor and Dean

&

Dr. S. THIRUMALINI

Associate Professor

School of Civil and Chemical Engineering

VIT University, Vellore- 632014

July 2016

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CONTENT

Chapter Description Page No.

1 Introduction 2

2 Methodology 13

3 Results and Discussions 29

4 Conclusions 72

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Chapter 1

INTRODUCTION

1.1 GENERAL

India has a finite number of very rich, and assorted cultural heritage in the form of built

structures and architectural monuments. Any structure that is of historical, archaeological or

artistic interest and existing for more than 100 years is called as an ancient monument. They

include different types of structures such as temples, palaces, domes, forts, ports, aqueducts,

prayer halls, cemeteries, step-wells, rock-cut temples and excavation sites. They are the proof

of ancient habitation and represent indigenous traditional architecture of India. They not only

represents the cultural face and growth but also articulate the knowledge of our ancestors about

building design, construction materials, building technology, creative and decoration and

artistic capabilities of the craftsmen (Nene2012).

Out of 125 heritage sites declared by UNESCO, 29 are in India. Currently,

3650 ancient monuments and archaeological sites have been declared as remains of national

importance. In Tamil Nadu alone, there are 248 structures and 163 prehistoric archaeological

sites. They are distributed in different geographical locations and belong to different periods,

ranging from early historic period to the colonial period. They also contribute to the prosperity

and economic wealth of our country. Only a small number of monuments are under the

protection of the state and central archeological survey of India and the remaining left

unnoticed.

As a result of this, finite, non-renewable and irreversible resources of our country are

fast disappearing without any record for the posterity. The main factors which lead to the non-

existence were lack of fundamental knowledge, understanding of construction of monuments,

interest in our past, lack of public awareness, industrial revolution and rapidly transforming

lifestyle, etc.

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1.2 REASONS FOR THEIR NON – EXISTENCE

Lack of fundamental knowledge

Understanding of construction of monuments

Interest in our past, lack of public awareness

Industrial revolution

Rapidly transforming life style

Finite, non-renewable and irreversible resources of our country is fast disappearing

without any record for the posterity

1.3 NEED FOR THE STUDY

The difficulty in understanding the old mortar could be attributed to the variety of raw

materials and organics used for their production and their application techniques.

Other parameters include the environmental conditions such as climate, humidity etc

which could influence their strength and durability.

It is the need of the hour to investigate the traditional construction material

characteristics and construction techniques for effective simulation, conservation,

protection and to safe guard our ancient monuments.

The present study could serve a great source of information regarding the type and

proportion of raw materials used (binder, aggregate and organic additives), their

application technology, as well as their resistance to ageing and environmental

conditions in the temples and also to prepare the compatibility mortar for conservation.

1.4 OBJECTIVES AND SCOPE OF THE STUDY

To identify the technology of production and characterize the raw materials of the

mortar used at Naganathaswamy Temple and Thanjavur Palace, Tamil Nadu.

To simulate the similar mortar by trial and error in the laboratory.

To find out the scientific reason beyond the durability over centuries and to evaluate its

compressive strength, water absorption, curing period carbonation and porosity for the

preparation of compatibility mortars for repair works.

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To validate the results of controlled and ancient samples by advanced analytical

techniques like X- Ray Diffraction, Scanning Electron Microscope with energy

dispersive X- Ray spectroscopy, Thermal Gravimetric Analysis, Fourier Transform-

Infra Spectroscopy.

1.5 ABOUT THE NAGANATHASWAMY TEMPLEAND THANJAVUR PALACE

1.5.1 Naganathaswamy Temple

The temple (Fig. 1) is 1000 years old is located in Manambadi near Kumbakonam. It is said

that the temple was built in tenth century by RajendraChola.The State government has ensured

the protection of 1,000-year old Naganathaswamy temple near Kumbakonam.

Fig.1 Naganathaswamy Temple

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1.5.2 Thanjavur Palace

Thanjavur Palace (Fig. 2) with its architectural beauty reflects the ‘Marathas’ and ‘Nayaks’

patronage towards art and culture. The tower is currently having seven storeys, but originally it

was having many number of storeys, which were damaged by thunder and rain. A research note

informs that there was a novel clock of sizable dimensions, forming part of the structure in

which the figure of a monkey used to strike the gong every hour. The tower is fashioned in the

style of Gingee Nayaks. It’s a protected monument by the State ASI department, located at

Thanjavur. It was constructed during the Nayaka and Maratiya periods.

Fig.2 Thanjavur Palace

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DESCRIPTION OF HERITAGE STRUCTURE

NAGANATHA SWAMY TEMPLE

INTRODUCTION

Naganatha swamy temple is a thousand years old temple built by Rajendra chola in Tanjavur

District. Rajendra Chola-I, was known as much for building temples as for extending his

empire to the banks of the Ganga in the north and to Srilanka and Maldives in the south. One

such small temple was the Naganathaswamy temple in Manambadi village near Kumbakonam

which has now virtually disappeared. The temple’s main deity is Lord Siva was initially known

as Sri Kailasamudaiyar temple.

The stone temple was built around 1016 CE, much before the king's masterpiece, the

Gangaikondaan temple, was raised. The temple is one of the 88 protected monuments in the

state under the control of the state department of archaeology. A sculpture in the

Naganathaswamy temple, where the Chola king along with his family is seen worshipping Lord

Nataraja, signifies the consecration of the temple during his period.

Epigraphist and historian Kudavayil M Balasubramaniam noted the temple has sculptures

depicting a story of an elephant and a spider that worships and protects a 'sivalinga' from leaves

falling on it. "A sculpture shows the Cauvery as a woman holding a lotus. The temple's flower

garden was called Rajendra Cholan.

The deities were called Sri Kailasamudiyar, while the village was called Ilachchikudi. The

sculptures depict dance dramas that used to be conducted during festivals in the Tamil month of

'Chithirai'. The State government's Archaeology Department declared it a protected monument

30 years ago. The stone structure below the vimana, with intricate sculptures, and the sanctum

sanctorum with a Siva lingam are intact. The temple has an entrance without a gopuram. The

prahara has flower plants.

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According to Kudavayil Balasubramanian, epigraphist and historian, this temple was

constructed by Rajendra Chola (1012-1044 AD). During Chola rule, the village was called

‘Elaichikudi’, and ‘Veeranarayanapuram’. The temple’s name was ‘Sri Kailasam’.

The temple possesses more than ten inscriptions of the Chola period. Some of the sculptures on

the walls of the main structure are those of Nataraja, which is an outstanding one. Another

sculpture depicting Rajendra Chola worshipping the Lord with his wives is seen. Other

sculptures depict Ganapathi, Dakshinamurthy, Ligotpava, Vishnu, Brahma, Gangadharamurthy,

Durga and Arthanari. Among Chola sculptures, they are the unique ones.

A) THANJAVUR PALACE

INTRODUCTION

The Thanjavur Maratha Palace Complex, known locally as Aranmanai, is the official

residence of the Bhonsle family who ruled over the Tanjore region from 1674 to 1855.The

Thanjavur Maratha palace was originally constructed by the rulers of Thanjavur Nayak

kingdom. After the fall of the Thanjavur Nayak kingdom, it served as the official residence of

the Thanjavur Maratha. When most of the Thanjavur Maratha kingdom was annexed to the

British Empire in 1799, the Thanjavur Marathas continued to hold sway over the palace and the

surrounding fort. The Bhonsle family continued to hold on to the palace even after the last

king Shivaji II was deposed as per the Doctrine of Lapse.

The palace complex consists of the Sadar Mahal Palace, the queen's courtyard and the Durbar

Hall. The Raja Serfoji Memorial Hall and the Royal Palace Museum are situated in the Sadar

Mahal Palace. There is also a small bell tower. The Saraswathi Mahal Library is situated with

the Thanjavur palace complex.

The original name of Thanjavur Palace is Sivaganga Fort, which is rarely used these days. If

you observe carefully, there is even a small moat around it which provided security against

enemy access. Often mistakenly called the "Thanjavur Maratha Palace" was not built by

Maratha Kings, but by Thanjavur Nayaks. However, the Marathas made some enhancements to

suit their needs.

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Thanjavur, formerly Tanjore, is a city in the south Indian state of Tamil Nadu. Thanjavur is an

important center of South Indian religion, art, and architecture. Most of the Great Living Chola

Temples, which are UNESCO World Heritage Monuments, are located in and around

Thanjavur. The foremost among these, the Brihadeeswara Temple, is located in the centre of

the city. Thanjavur is also home to Tanjore painting, a painting style unique to the region.

GEOGRAPHY AND HISTORICAL DEVELOPMENT OF THE LOCATION

The Thanjavur Maratha Palace is located in Thanjavur. Thanjavur is the headquarters of

the Thanjavur District. The city is an important agricultural centre located in the Cauvery

Delta and is known as the "Rice bowl of Tamil Nadu". Thanjavur is administered by

a municipal corporation covering an area of 36.33 km2 (14.03 sq mi) and had a population of

222,943 in 2011. Roadways are the major means of transportation, while the city also has rail

connectivity. The nearest airport is Tiruchirapalli International Airport, located 59.6 km

(37.0 mi) away from the city. The nearest seaport is Karaikal Port, which is 94 km (58 mi)

away from Thanjavur.

While the early history of Thanjavur remains unclear, the city first rose to prominence during

the reign of Medieval Cholas when it served as the capital of the empire. After the fall of

Cholas, the city was ruled by various dynasties likePandyas, Vijayanagar Empire, Madurai

Nayaks, Thanjavur Nayaks, Thanjavur Marathas and the British Empire. It has been a part of

independent India since 1947.

Thanjavur became the most important city in the Chola Empire and remained its capital till the

emergence of Gangaikonda Cholapuram in about 1025 During the first decade of the eleventh

century, When the Chola Empire began to decline in the 13th century, the Pandyas from the

south invaded and captured Thanjavur twice, first during 1218–19 and then during 1230.

During the second invasion, the Chola king Rajaraja III (1216–56) was set in exile and he

sought the help of the Hoysala king Vira Narasimha II (1220–35) to regain

Thanjavur. Thanjavur was eventually annexed along with the rest of the Chola kingdom by the

Pandya king Maravarman Kulasekara Pandyan I (1268–1308) in 1279 and the Chola kings

were forced to accept the suzerainty of the Pandyas. The Pandyas ruled Thanjavur from 1279 to

1311 when their kingdom was raided and annexed by the forces of Malik Kafur (1296–1306)

and Delhi Sultanate. The Sultanate extended its authority directly over the conquered regions

from 1311 to 1335 and then through the semi-independent Ma'bar Sultanate from 1335 to 1378.

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Starting from the 1350s, the Ma'bar Sultanate was steadily absorbed into the rising Vijayanagar

Empire.

Fig 2.1 Thanjavur Royal Palace courtyard

Thanjavur is an important pilgrim centre and a major tourist destination of Tamil Nadu. South

Zone Culture Centre in Thanjavur is one of the regional cultural centres established by the

Government of India to preserve and promote cultural heritage of India. There were 2,002,225

Indian and 81,435 foreign tourist arrivals in 2009 to Thanjavur. The Thanjavur Maratha

palace was the official residence of the Bhonsle family who ruled over the Thanjavur region

from 1674 to 1855. It was originally constructed by the rulers of Thanjavur Nayak

kingdom and after their fall, it served as the official residence of the Thanjavur

Marathas. When most of the Thanjavur Maratha kingdom was annexed by the British Empire

in 1799, the Thanjavur Marathas continued to hold sway over the palace and the surrounding

fort. The southern side of the third quadrangle of the palace has 190 ft (58 m) tower like

building, called the Goodagopuram.

The Saraswathi Mahal Library, established around 1700 and located in the premises of the

palace, contains over 30,000 Indian and European manuscripts written on palm leaf and

paper. Over eighty per cent of its manuscripts are in Sanskrit and many of them are on palm

leaves. The Tamil works include treatise on medicine, and commentaries on Sangam

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literature. The Rajaraja Chola art gallery is located inside the palace – it has a large collection

of stone and bronze images from the ninth to 12th centuries. Most of the idols present in the

gallery were collected from various temples in the Thanjavur district.

Fig. 2.2 Depicting a Thanjavur painting

Schwartz Church, a historic monument located in the palace garden, was built in 1779

by Serfoji II as a token of affection for Rev. C.V. Schwartz of the Danish Mission. There are

five museums in the city namely Archeological Museum, Tamil University Museum located

with the Tamil University premises, the Saraswathi Mahal Library Museum located inside the

Saraswathi Mahal, Nayak Durbar Hall Art Museum and Rajaraja Chola Museum. Raja Rajan

Manimandapam is one of the tourist attractions in Thanjavur, built during the Thanjavur Tamil

Conference in 1991. "Sangeetha Mahal" has a permanent handicrafts exhibition centre.

Thanjavur is the cradle for many of the arts and crafts in South India. Carnatic musicwas

codified in Thanjavur and the art flourished during the Nayak rule in the 16th century.

Brief History of the Palace

After the fall of Cholas in 1279 A.D, and a few centuries of Pandyan occupation, Sevappa

Nayak captured Thanjavur and became the King in 1532. The construction of Thanjavur Palace

began in 1534 and was completed in 1535, thanks to plenty of local prisoners of war who

provided manual labor. The Palace was officially called "Sivagangai Fort" and was held by the

Nayak family until April 1674, when the Maratha ruler Venkoji captured it. The Marathas

enhanced the original structure and expanded the palace complex. It was used by them until

1799 when British finally annexed the Thanjavur Maratha Kingdom.

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Plenty of tourists expect a gigantic, luxurious and ornamented interior and get disappointed.

The complex was built as a fort, not a palace. The Nayaks chose the site carefully and there is

even a moat around the complex to protect it. Another intriguing feature is the extremely

narrow staircases with short steps, sharp turns and low ceilings. Why would a palace have such

primitive staircases? This was a measure to prevent enemies' rapid advance. Cavalry advances

would be impossible through the stairs, and the foot soldiers cannot climb up with great speed.

The enemy foot soldiers would be easy prey to the men waiting for them above. Again: this

was built as a fort, not a palace.

Secret Chambers:

There are at least 3 hidden chambers with secret, interconnecting doors. These were used as

torture chambers and to have discreet meetings. One hidden chamber, located at the base of the

Arsenal tower is acoustically designed in a way that you can hear even the smallest whisper

from 3 floors above. This must have been used as a way for sending secret voice signals over

multiple floors. Sadly, the Government has completely prohibited all access to these hidden

chambers.

Underground Tunnel:

There are two underground passages in the palace, only one of them is partially accessible by

tourists. This is a relatively short passage and the Government is renovating it as of 2014.

Another secret tunnel which is a mile long, connects the Brihadeeswara temple and the palace.

It is wide enough to ride 2 horses in parallel, and was designed as a getaway route by Kings

during war times.

Arsenal Tower (Koodagopuram):

This is a 192 feet tall pyramidal structure with eight floors. The initial building was constructed

by Nayaks in 1645 with only 2 floors. The Marathas later renovated and finished the tower in

1855, and used it for various military purposes. The top floor was used as a watch tower, and

the remaining floors were used to store arms and ammunition. The second floor was

exclusively used for the King's martial arts training.

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Fig. 3 The Arsenal Tower at Thanjavur Palace

Bell Tower (Maadamaaligai):

Fig. 4 The Bell Tower was once used as a clock tower (just hourly bells) by locals

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Chapter 2

METHODOLOGY

2.0 GENERAL

The entire experimental works were carried out in two phases:

Part 1: Characterization of ancient mortar for both locations

Part 2: Simulation of repair mortar

PART 1: CHARACTERIZATION OF ANCIENT MORTAR FOR BOTH LOCATIONS

2.1 REVERSE ENGINEERING METHODOLOGY

The reverse engineering methodology was followed to characterize the ancient mortars as

given in following steps:

Step1: Characterization of historic mortars

Step 2: Selection of raw materials

Step 3: Preparation of mortars

Step 4: Experimental investigation

Step 5: Optimization – Standardization

Step 6: Pilot application of restoration mortars

2.2 CHARACTERIZATION OF HISTORIC MORTARS

Step 1 : Sampling

Step 2 : Chemical analysis

Step 3 : Acid loss analysis

Step 4 : Granulometry of sand

Step 5 : Mineralogical analysis

Step 6 : FT-IR

Step 7 : TGA with DTA

Step 8 : Texture analysis

Step 9 : Organic test

Step 10 : Interpretation of results

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2.2.1 Sampling of Mortar

The location for sampling was selected. The analyses were carried out in a significant quantity

of samples in order to avoid errors caused by heterogeneity. Samples were taken from the

upper parts of the temple to avoid such phenomena caused by capillary rise. Altered (decayed)

and non-altered material samples were taken from both internal and external portion of the

temple. Samples nearer to decay portion and cracks were avoided.

Sufficient number of samples (min. 15 samples) shown in Fig. 3 and 4 from temples were taken

for the study. Analysis of these samples showed details about the original as well as the

degraded mortars. The samples are grouped based on their similar characteristics.Table 1 and

2 lists the sampling points from Naganathaswamy Temple and Thanjavur palace.

A

B

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Fig 3 : A) Main Mandabam Top Dome B) East Entrance left side C) Person collecting

the sample D) Inner portion of the wall of the Naganathaswamy Temple

Table.1 Sample identification at Naganathaswamy Temple

S.No Sample Name Type of Mortar Location

1 N.S-1 Plastered Mortar East Entrance left side

2 N.S-2 Bedding Mortar Entrance wall

3 N.S-3 Bedding Mortar Compound wall East

4 N.S-4 Plastered Mortar Compound wall Out side

5 N.S-5 Bedding Mortar Main Mandabam

6 N.S-6 Plastered Mortar Near Vinayagar statue

7 N.S-7 Bedding Mortar Main Mandabam Back Side

8 N.S-8 Bedding Mortar Small Mandabam SW corner

9 N.S-9 Plastered Mortar West small Mandabam

10 N.S-10 Bedding Mortar Small Mandabam NW corner

11 N.S-11 Bedding Mortar Main Mandabam North facing

12 N.S-12 Bedding Mortar Vinayagar Temple inner Dome

13 N.S-13 Flooring Mortar Main Mandabam inner Flooring

14 N.S-14 Bedding Mortar Main Mandabam Beam

15 N.S-15 Plastered Mortar Main Mandabam Top Dome

C D

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Sample identification – Thanjavur Palace

Fig. 4 A) Museum Outer Wall,

B) SaraswathimahalEntrance,

C) Collection of the sample by the

Investigator,

D) Bell tower

E) Durbar north side arch wall

A B

C D

E

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Table 2 Sample identification at Thanjavur Palace

S.No Sample Name Type of Mortar Location

1 T.P-1 Mud Mortar Back to Amman Statue

2 T.P-2 Bedding Mortar Near Library

3 T.P-3 Plastered Mortar Durbar entrance

4 T.P-4 Bedding Mortar Arch/Durbar hall

5 T.P-5 Bedding Mortar Bell tower / First floor

6 T.P-6 Bedding Mortar Elephant tieng place

7 T.P-7 Plastered Mortar Arch/Ticket counter

8 T.P-8 Plastered Mortar Museum entrance

9 T.P-9 Plastered Mortar Side wall / JE office

10 T.P-10 Plastered Mortar Bell tower / Outer wall

11 T.P-11 Bedding Mortar Library entrance

12 T.P-12 Bedding Mortar North wall/ Durbar hall

13 T.P-13 Plastered Mortar Inner wall / JE office

14 T.P-14 Plastered Mortar First floor / Durbar hall

15 T.P-15 Plastered Mortar Inside arch / Ticket counter

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2.2.2Acid loss Test

The dissolution of the mortar in hydrochloric acid yielded three fractions: Insoluble

fraction/soluble fraction from calcium content, clay minerals and volatile fraction.

2.2.3 Organic Test

The presence of fat, protein in both ancient and new mortars were tested using Lane &Eynon

method. The presence of carbohydrate was calculated by Kjeldhal method.

2.2.4 Chemical Analysis

Samples (Table 3) were analysed for their chemical composition by adopting traditional

method of testing. CaO and MgO were quantified on titration with ethylene diamine tetra acetic

acid (EDTA), using eBT as indicator. The amounts of Al2O3and Fe2O3 were determined by

Atomic Absorption Spectroscopy (AAS). Gravimetric method was used to find the amount of

silica present. The hydraulic index (HI) and cementation index (CI) were calculated

[Taylor,1990 Boynton,1980]

Table 3 Tests for Chemical Analysis

S.No Minerals Method employed

1. CaO+ MgO Titration Method

2. Al2O3& Fe2O3 Atomic Absorption Spectroscopy ( AAS)

3. SiO2 Gravimetric Method

4. K, S Gravimetric Method

5. Na and Cl Titration Method

6. LOI Using Muffle furnace

HI = (%Al2O3+ % Fe2O3 + % SiO2) / (% CaO + % MgO) , If 0.3 < HI < 0.5 Weakly

Hydraulic, 0.5 < HI < 0.7 Moderately Hydraulic , 0.7 < HI <1.1 Eminently hydraulic

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CI = (1.1%Al2O3+ 0.7% Fe2O3 + 2.8 % SiO2) / (% CaO + % MgO)

If 0.3 < CI< 0.5 Weakly Hydraulic, 0.5 < CI < 0.7 Moderately Hydraulic

0.7 < CI<1.1 Eminently hydraulic ,Highly hydraulic Higher the index , more

hydraulic properties.

2.2.5 Binder -Aggregate Ratio

The raw material composition was found by dissolving the carbonated lime in 10 % of

hydrochloric acid, leaving out fine aggregates.

2.2.6 Electronic Particle Size Analyser

The particle size distribution was carried out and grading was done.

2.2.7 Organic Test

The herbs used in preparation of lime mortar was tested for the presence of carbohydrate,

protein and fat.

2.2.8 Analytical Techniques

The analyses of ancient mortars were done using following instrumental techniques.

XRD analysis of finely ground samples was done using Bruker Desktop-Diffracometer

working with the Cu Ka radiation and interpretation by Bruker DIFFRAC.SUITEEVA

Software.

Thermal Gravimetric Analysis (TGA) was performed to find the hydroscopic and structural

bound water content of lime mortar and it is also helpful to determine any possible thermal

decomposition of mineral phases. Here weight loss of sample was monitored as a function of

temperature. TGA could serve as best tool to characterize and evaluate historic mortars.

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DTA reveals thermal transformation of various components heated under controlled conditions.

The phase transfers are exothermic or endothermic in nature. DTA was carried out on non-

fractioned mortar to find the dehydration, oxidation and decomposition

Infrared Spectroscopy (FT-IR analysis) provides supplementary information to XRD. It is

mainly carried out to identify the presence of organics in the mortars.

SEM (FEI Quanta FEG 200) was used to determine the surface morphology of the mortars,

specially cracks and pores of the samples. SEM images revealed the mineral morphology of

hydrated phases.

EDX was used to unveil the elemental composition of mortars.

PART- II SIMULATION OF REPAIR MORTAR

The objective of the work is to simulate the similar mortar by trial and error in the laboratory

and to evaluate its compatibility.

2.3 MATERIALS USED

2.3.1 Lime

Mortars were prepared using commercial natural hydraulic lime. Lime was purchased from

Pollachi, Coimbatore that is being used widely in the restoration works. Lime used in the study

is a uniform material manufactured by an industrial process. It was obtained by ignition of the

regionally available limestone. The lime was slaked in a traditional manner in huge vats. After

sieving to remove larger and unslaked particles, it was left to settle for one month before being

transferred to 25 Kg plastic bags. The lime has a particle size of 850 microns below to be used

in lime mortar.

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2.3.1.1 Chemical characteristics of lime

There is a varied geological distribution in India. Hence several kinds of lime stones are

available. These lime stone are burnt to obtain building lime. Due to the variability of limestone

from place to place, the resulting lime is expected to vary in quality. Hence, chemical

characteristics were carried out as per IS: 6932 (Part V) - 1973. The hydraulic lime used for

investigation was subjected to preliminary chemical analysis by Atomic Absorption

Spectrometry (AAS) and gravimetric method. Oxides such as calcium oxide and magnesium

oxide, silica, alumina and ferric oxides were determined to identify the class of the lime and to

assess the hydraulicity of lime.

2.3.1.2 Physical characteristics of lime

Field tests on building lime

Lime is a reactive material and constantly undergoes chemical changes on exposure to the

atmosphere. Even during manufacture there are chances of variability in the quality. Therefore,

it is necessary to check the quality of lime at various stages. For quick and reliable results

simple field tests on lime such as visual examination, ball test, and hydrochloric acid test have

been done as per IS: 1624- 1986.

(a) VISUAL EXAMINATION

Lime was examined for color and state of aggregation namely lumpy, powdery, soft or hard.

Class C lime and class D lime mostly used for white washing are white in color. Lumpy form

may indicate quicklime or unburnt limestone. Lime free from coarse and gritty pieces larger

than about 2.30 mm may be categorized as Class ‘A ‘ lime.

(b) BALL TEST

Ball test was conducted as per IS: 1624 – 1986, where lime was sieved through 850

microns sieve. Then the lime was mixed with sufficient quantity of water to get a stiff paste and

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a ball of 50 mm diameter was prepared and it was left undisturbed for a period of six hours.

Then the ball was gently immersed in a jar of water.

The codal guidelines for assessing the class of lime is as follows.

No signs of disintegration - Class A lime

Very little expansion and numerous cracks - Class B lime

Signs of disintegration within few minutes - Class C or Class D lime

(c) HYDROCHLORIC ACID TEST

The test was conducted as per IS: 1624 - 1986. Lime was examined to find out the presence of

inert material. Sufficient quantity of lime was placed into a 50 ml glass cylinder up to 5 ml

mark. Twenty five ml hydrochloric acid was added into the cylinder along the glass rod placed

inside so that the acid does not get smeared all over the sides of the cylinder. The contents were

stirred with a glass rod. The cylinder was left with the contents for 24 hours to observe the gel

formation.

SETTING TIME OF LIME

Initial and final setting times of lime have been determined according to IS: 6932 (Part 11) -

1973 by using Vicat apparatus. Initial setting time is defined as the time measured from mixing

binder with water to the time at which the needle fails to pierce the binder paste (5 ± 1) mm

from the base-plate. Initial setting time needle was replaced by an annular arrangement for the

determination of final setting time. The lime is considered as finally set when the needle

applied on the surface of test block fails to make an impression.

2.4 SAND

Sand is used as an aggregate in mortars, plasters and renders. The properties of sand used in the

mix have a major effect on its workability, final strength and durability.The quality of sand is

of primary importance in achieving a high-quality lime mortar. Sand provides the structural

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strength, with the lime putty coating and cementing the particles together. In this investigation,

clean river sand free from organic and inorganic particles were used as aggregates in mortar

preparation.

2.4.1 Grain size distribution

Grain size distribution of sand have been determined as per IS: 2386 (Part 1) - 1963 on

mechanical sieve shaker with sieve series (square mesh) of size 2.36 mm, 1.18 mm, 0.6 mm,

0.3 mm, 0.15 mm and 0.075 mm, with sieving time of 10 minutes. Individual fractions were

weighed, and the results were plotted.

2.5PREPARATION OF MORTAR SPECIMENS

A mix proportion of 1:3 (1 part of hydraulic lime, 3 parts of sand) by weight was chosen which

has been considered as the most common mix proportion for restoration works (Moropoulou et

al., 2003). Hydraulic lime mortars were prepared as per Indian standards IS: 6932 Part VII –

1973. Equal quantities of hydraulic lime and water were thoroughly mixed for five minutes

(lime putty). The hydraulic lime putty so prepared was mixed with sand and then ground for a

period of 8 minutes and then left aside for 24 hours. The (water + AN)/lime ratio was adjusted

to 0.65 at the time of casting. The prepared mortar mixtures were filled into non-corrosive

moulds of dimension 50x50x50 mm cube for compression tests and 40x40x160 mm prism for

flexure tests and gently pressed using the thumb. Steel moulds with zinc coating were used for

this purpose to avoid corrosion. The filled up moulds were covered with wet cloth and

maintained at a temperature of 27±2 º C, and 90 percent RH. Samples were demoulded after 3

days and kept in air for a further period of 4 days at the same temperature and humidity to

avoid cracks due to drying shrinkage. Thus the cubes of seven days old were immersed in clean

water and left till the prior date of testing for its strength in UTM. The water should be

periodically changed for every 3 days and maintained at a temperature of 27 ± 2°C.

24

Fig 5 Preparation of Mortar Mix

Fig 6 curing of casted specimens

2.6 CONSISTENCY TEST ON LIME MORTAR

The typical consistency of a Lime paste is the consistency, which will permit the Vicat plunger

to penetrate to a point 5 to 7 millimeter from the bottom of the mould. Lime and water of

weighted quantity is taken and made as paste, taking care that the time of mixing was not less

25

than three minutes nor more than five minutes and the gauging is completed before any sign of

setting occurs. The time should be noted immediately after the water is added to the lime. Then

the vicatmould is filled up with this paste in three layers, compacting each layer by keeping the

mould on a non-porous glass plate and the top surface is smoothened. This whole set up is then

placed under the plunger so that it touches gently on the surface of the paste and it is released at

once so that it penetrates into the paste. This operation was repeated for different trial mixes

and the consistency was found.

2.7 SETTING TIME ON LIME MORTAR

Initial and final setting times of lime were done as per IS: 6932 (Part 11) – 1973 [11] by using

Vicat apparatus. Initial setting time is the time taken for the needle, which fails to penetrate the

binder paste (5 ± 1) mm from the base-plate. The final setting time was founded out by

replacing the needle by an annular arrangement. The lime was identified as finally set when the

needle fails to make an impression on the surface.

2.8 COMPRESSIVE STRENGTH TEST

The compressive strength test was conducted as per IS: 6932 (Part VII) – 1973 [12]. Three

cubes are taken out from water after 28 days and wiped out so that its surface gets dried.

Keeping those cubes in the low capacity compression-testing machine tests the compressive

strength of these cubes. The casted face should be facing towards the person. The moulded side

should be in contact with the surface through which load is applied. There should not be any

packing between the cube and steel plates of the testing machine. The top steel platen is fixed

with ball bearing and shall be self-adjusting. The load should be stable and uniformly applied,

starting from zero increasing at the rate of 15 kg/min. The average strength of the six

specimens shall be taken as the compressive strength of the mortar and the result expressed in

N/mm2.

26

Fig. 7 Compressive strength test for the specimen

2.9 FLEXURAL STRENGTH TEST

The determination of flexural strength is undertaken when the test specimens are twenty-eight

days old, the testing machine is required to have two supporting rollers and a third roller (the

loading roller, located above the test specimen and midway between the supporting rollers).

The prism is placed so that one of its faces, which has been cast against the steel mould, is in

contact with the supporting rollers. The load is applied to the test specimens at a rate that

produces failure in a time period of thirty to ninety seconds. The load at failure was noted.

Fig. 8 Flexural strength test for the specimen

27

2.10 WATER RETENTIVITY TEST

This test determines the change in the level of consistence when the mortar is subjected to

suction and the loss of water from the fresh mortar. The mould of 10 cm internal diameter and

2.5 cm height is weighed and eight discs of filter paper are also weighed. The mould is then

filled with lime mortar and the top surface is the leveled with the palette knife. The mould and

its contents are then weighed.

The eight discs of filter paper are placed on top of the mortar and a non-porous plate is placed

on top of these together with a 2 kg weight. A period of two minutes is allowed to elapse, the

weight and plate removed, the cotton gauze discarded and the filter papers weighed to the

nearest 0.05 grams.

The mass of water remaining in the mould (i.e. the mass of water originally in the mortar minus

the water absorbed by the filter paper) is expressed as a percentage of the original water content

of the fresh mortar and reported as the water retentivity.

2.11 BULK DENSITY AND POROSITY INFLUENCE

The bulk density (Rilem TC 203 2009) is the ratio of the mass of the mortar to its bulk volume.

It is calculated as ratio of 28th day weight of the sample to its volume. Porosity is indirect

measure of water absorption and easy measure of carbonation. It is defined as the fraction of

the total volume of a solid that is occupied by pores or empty spaces or voids. It is calculated

based on Archimedes principle (RilemTC 25 1980).

The samples were initially dried at 103 ºC for 24 hours and weighed to determine their dry

weights (Md). Then the samples were immersed in water for 24 hours and weighed Ms. Also the

Archimedes weight of the mortar sample, immersed in water (Ma) was measured. Bulk density

and porosity was calculated using Eqn 3.4 and Eqn 3.5

Equ.3.4

28

Porosity of the mortar was calculated using Eqn. below

Equ.3.5

Where

D - Bulk Density (g/cm3)

Md- Dry mass (g)

Ms- Saturated mass (g)

Ma- Archimedes mass (g)

2.12 CAPILLARY ABSOPTION

Sasse and Snethlage [1997] observed that the water transport characteristics of the mortar and

substrate must be similar to avoid differential discolouration over time and strong weathering

along the contact zones. In addition to this, these properties exert an influence on deterioration

mechanisms such as salt crystallization and freeze-thaw, which are the result of the movement

of water into, through and out of stone [Russell et al, 2002]. Bromblet [2000] used these tests to

make comparisons between mortars and stones in order to assess compatibility following the

Sasse & Snethlage precepts. The presence of large pores confers resistance to freezing since

they provide space into which ice crystals can expand without causing damage [Balksten&

Magnusson, 2004]. It is found by using

Where, C – Capillary absorption

m90 – Weight of sample after 90 min (g)

m10 - Weight of sample after 10 min (g)

29

Chapter 3

RESULTS AND DISCUSSSIONS

3.1 SAMPLE PREPARATION

The collected samples (Fig. 9) are crushed with mild pressure in hand and sieved through 63µm

sieve. The lime particles passing thorough sieve will be binder rich content is collected. The

acid loss analysis was carried on this portion.

Fig.9 Altered and Unaltered lime mortar samples

30

Fig. 10 Rich binder less than 63µm

3.2 Acid Loss analysis

The results of acid loss analysis of Naganathaswamy Temple and Thanjayur palace is

presented in Table 6 and 7 respectively. Binder to aggregate ratio of 1:3 to 1.6 for

Naganathaswamy Temple and in the range of 1:3 to 1: 7 for Thanjayur palace, respectively.

The palster of both the structures rich binder to aggregate ratio of 1:3 and bedding mortars

have lean ration for 1: 6.

31

Fig 11: Acid loss Test

Table 6 Acid Loss Analysis of Naganathaswamy Temple

Sample Initial

weight (gm)

Weight of sand

retained (gm)

Weight of

binder (gm)

B/A Ratio

1 28.65 24.29 4.35 1 : 5.6

2 31.41 27.12 4.28 1 : 6.3

3 24.85 19.40 5.44 1 : 3.5

4 26.75 21.67 5.07 1 :4.3

5 28.22 24.40 3.81 1 : 6.4

32

6 24.46 18.95 5.50 1 : 3.4

7 25.63 21.59 4.03 1 : 5.3

8 21.85 16.48 5.37 1 : 3.1

9 23.40 18.16 5.23 1 : 3.5

10 24.32 18.50 5.81 1 : 3.2

11 32.05 26.71 5.33 1 : 5

12 26.42 19.85 6.56 1 : 3.1

13 28.71 21.96 6.74 1 : 3.3

14 27.32 21.58 5.73 1 : 3.7

15 28.85 23.20 5.64 1:4.1

Table 7 Acid Loss Analysis of Thanjavur Palace

Sample Initial

Weight (gm)

Weight of sand

retained (gm)

Weight of

binder (gm)

B/A Ratio

1 28.66 23.211 5.449 1 : 4.26

2 25.51 20.95 4.56 1 : 4.6

3 27.41 24.115 3.295 1 : 7.32

4 24.98 19.069 5.911 1 : 3.23

5 25.57 20.086 5.484 1 : 3.66

6 26.46 22.559 3.901 1 : 5.78

7 24.75 20.33 4.42 1 : 4.6

8 27.04 23.748 3.292 1 ; 7.2

33

9 22.82 18.38 4.44 1 : 4.14

10 19.54 16.73 2.81 1 : 5.9

11 26.55 21.587 4.963 1 : 4.35

12 24.68 20.835 3.845 1 : 5.42

13 26.45 22.252 4.198 1 : 5.3

14 26.51 22.991 3.519 1 : 6.5

15 23.46 19.525 3.935 1 : 4.96

3.3 Chemical analysis of mortar samples

The complete characterisation of representative samples from each category is established.

Table 8includes the results of chemical analysis of all groups. Calcium carbonate (calcium

oxide and calcination loss) and silica were the main components identified. Presence of clay

minerals (Al2O3and Fe2O3) along with silica around 30% in the mortar samples indicates the

hydraulic nature of the lime. The percentage of silica content is highest whereas magnesium

content is minimum. Further, the hydraulic and cementation indices of all the ancient samples

are on the higher side and ranged from 1.39 to 1.7 and 3.6 to 6, respectively. As per Taylor

(1997) findings, the values proved that the lime powder used is similar to cement.

Table 8 Percentage of various minerals present in ancient lime mortar

(Naganathaswamy Temple)

Sample CaO

MgO

S cl Fe2O3

Al2O3

SiO2

Na

k

LOI

NS-1 33.41 27.22 9.51 8.16 10.43 5.18 3.21 2.14 0.74 19.21

NS-2 31.28 38.46

11.58 7.51 9.64

4.61 2.82 1.12 065 21.63

NS-3 34.74 22.95 12.18 9.25 8.54 5.21 3.61 3.13 0.34 18.33

NS-4 39.35 18.51 10.68 11.2

1 6.84

6.43 3.52 2.89 0.57 18.91

34

NS-5 28.35 23.64 13.51 8.34 11.15 9.83 2.16 1.89 1.08 22.04

NS-6 31.93 19.55 12.87 10.6

9 7.22

11.61 3.28 2.14 0.68 17.47

NS-7 26.27 29.31 9.24 9.37 8.31 7.11 5.92 3.53 0.94 19.07

NS-8 40.15 12.51 13.81 11.6

3 9.14

4.62 4.33 2.72 1.12 21.73

NS-9 33.43 16.65 14.29 10.2

7 12.51

6.46 4.08 1.83 0.52 20.69

NS-10 43.14 10.86 8.33 12.1

7 9.43

8.38 5.19 1.68 0.79 19.76

Table 9 Percentage of various minerals present in ancient lime mortar

(Thanjavur Palace)

Sample CaO

MgO

S Cl

Fe2O3

Al2O3

SiO2

Na

k

LOI

TP-1 44.56 11.51 8.91 11.14 9.09 7.61 5.19 1.39 0.55 31.24

TP-2 36.32 11.12 9.53 15.89 10.89 9.76 4.65 1.02 0.79 33.61

TP-3 42.95 13.25 7.65 11.2 11.57 7.84 4.01 1.27 0.46 25.71

TP-4 49.15 13.38 10.33 6.77 7.28 6.95 4.41 1.11 0.59 29.22

TP-5 37.98 14.07 8.27 15.64 8.71 8.26 5.47 1.05 0.58 35.47

TP-6 36.06 12.68 9.7 14.92 9.45 10.94 4.47 0.99 0.74 21.53

TP-7 39.69 12.56 9.04 15.43 8.59 7.93 4.63 1.554 0.55 23.81

TP-8 41.13 15.14 7.15 9.33 12.01 9.66 3.98 1.37 0.68 28.91

TP-9 43.39 10.38 5.45 18.69 9.27 6.96 4.13 1.12 0.56 26.06

TP-10 47.49 12.55 6.76 14.26 7.81 4.74 4.41 1.27 0.67 31.75

3.3 Organic analysis of mortars

The organic analysis of mortars samples are presented in Table 10 and 11, respectively for

Naganathaswamy Temple and Thanjayur palace. The percentage of carbohydrate is high in

both mortar with around maximum 3 % of protein and fraction of fats in the ancient samples.

Hence the kadukai and jaggery would have been added to the mortars to improve the fresh and

hardened properties of the mortar.

35

Table 10 Organic Tests on Naganathaswamy Temple

Samples Name Carbohydrate Fat Protein

1 N.S-1 5.02 0.07 0.58

2 N.S-3 0.33 0.04 2.69

3 N.S-9 6.16 0.06 0.39

4 N.S-11 6.67 0.08 0.96

5 N.S-17 9.78 0.13 0.26

Table 11: Organic test on Thanjavur Palace

Samples Name Carbohydrate Fat Protein

1. T.P-7 6.81 0.05 0.36

2. T.P-10 9.24 0.28 3.37

3. T.P-13 10.66 0.16 1.43

4. T.P-14 5.43 0.03 0.16

5. T.P-15 12.69 0.18 1.12

Kadukai or TerminaliaChebulashown in Fig.12 contains tannic acid or tannins made up of

polyphenoliccompounds which has ability to build very complex chemical structures. The

36

tannic acid has an estimated chemical formula of C76H52O46.Amala et al (2014) established that

the main composition is carbohydrates in the form of tannins.The basic unit of kadukai(tannin)

is in the form of gallicacidmay be natural or synthetic. The vegetable tannin or natural organic

tannins or sometimes even called as tannoid is a type of bio molecule whereas modern

synthetic tannin is an astringent. The polyphenolic compound present in the bitter plant binds

with lime and precipicate protein and various other organic compounds including amino

acids and alkaloids.

Fig.12 Dry seeds of Kadukai

Jaggery shown in Fig 13 is an amorphous form of unrefined and non-distilled sugar prepared

from sap or juice of plants that contains sugar. The addition of jaggery to lime, increases the

solubility of lime in water by 84%. Hence, instead of water jaggery extract water can be added

during slaking. This helps in more conversion of calcium oxide (lime) into calcium hydroxide

(portlandite). Jaggery contains 60 - 85 % sucrose, 5-15% glucose and fructose, 0.4% protein

and 0.6 – 1 % of minerals.

37

Fig.13 Jaggery from sugar cane

3.4 SIEVE ANALYSIS OF NAGANATHASWAMY TEMPLE

Sieve analysis (Table 12 and 13, Fig. 14 to 19) indicates the uniform graded particles unlike

well graded particles. Hence grinding was done to overcome the short comings of improper

slaking and to improve the pozzolanic activity of lime with clay minerals. Slaking was carried

out during manufacturing of lime. The process of adding and mixing of water to lime is called

slaking which may be wet or dry. In dry slaking less amount of water is added to lime that

cause conversion of partial amount of lime into portlandite. It is preferred when quality of

water is poor or insufficient for use. However, in wet slaking in excess of water when carried

for long duration lasting up to months, the complete transformation of calcium oxide into

portlandite is possible. Moreover, wet slaking will prevent carbonation, the portlandite crystals

formed changes its shape, become smaller and flatter. This allows the crystals to move easily

on other crystals thus aiding workability (Sangeethabais2007). During the process of slaking, a

lot of heat was generated which causes the lime to split. This process will not happen in case of

improper slaking as the parameters required for lime production were not standardized

resulting in large variations at each source point. Hence, grinding is necessary. Though slaked

lime was procured for production, minimum grinding was carried out to ensure the two things

to happen. By grinding,splitting of lime takes places and the silica grains become finer in order

of nanometers. Fine silica and clay minerals accelerate the reaction rate less than a day to form

38

CSH phases without changing the microstructure of lime matrix (Moropoulou et al

2004).Without grinding the mortars will take much time to reach the similar extent of reaction.

Similarly, micronized lime will result in change in shape of portlandite for good workability.

Fig.14 Sieve analysis of NS – 6

Fig.15 Sieve analysis of NS – 8

39

Fig. 16 Sieve analysis of NS – 10

Fig. 17 Sieve analysis of TS– 6

40

Table 12 Sieve analysis of Naganathaswamy Temple

Sample Total 4.86 2.8 2.36 1.4 600 425 300 150 90 75 Pan

N.S-1 24.296 Nil Nil Nil 0.154 3.217 4.347 5.637 8.271 2.173 0.06 0.437

N.S-2 27.124 Nil Nil 0.23 0.6 3.4 5.332 6.714 8.457 1.955 0.09 0.346

N.S-3 19.407 Nil Nil Nil 0.224 1.001 1.485 2.607 5.72 4.725 0.309 3.336

N.S-4 21.672 Nil Nil 0.498 1.655 3.543 2.787 2.936 5.456 3.098 0.366 1.333

N.S-5 24.409 Nil Nil 0.1 0.16 2.026 7.29 7.749 5.155 1.52 0.105 0.304

N.S-6 18.955 Nil Nil Nil 0.042 0.877 2.926 4.917 7.823 1.688 0.105 0.577

N.S-7 21.596 Nil Nil Nil 0.102 1.341 3.627 5.767 7.89 2.183 0.143 0.543

N.S-8 16.48 Nil Nil Nil 0.11 5.04 0.031 4.516 5.004 1.398 0.075 0.306

N.S-9 18.169 1.53 0.356 1.653 2.522 1.834 1.253 1.406 4.448 2.398 0.109 0.66

N.S-10 18.505 Nil Nil 0.208 0.575 1.878 3.381 4.41 6.018 1.533 0.071 0.431

N.S-11 26.719 1.25 Nil 1.102 0.031 1.52 6.242 4.615 8.325 2.612 0.658 0.364

N.S-12 19.855 Nil Nil 0.541 1.022 2.321 3.043 5.168 4.346 1.932 0.246 1.236

N.S-13 21.965 Nil 0.265 Nil 1.406 3.245 2.846 2.845 6.826 3.421 0.365 0.746

N.S-14 21.588 0.85 Nil 0.109 0.184 1.336 5.212 3.965 4.183 2.667 0.614 2.468

N.S-15 23.209 Nil Nil Nil 1.865 3.452 6.328 2.725 7.098 1.064 0.245 0.432

41

Fig. 18 Sieve analysis of TS– 7

Fig. 19 Sieve analysis of TS– 9

42

Table 13 Sieve Analysis of Sand (Thanjavur Palace)

Sample Total 4.86 2.8 2.36 1.4 600 425 300 150 90 75 Pan

T.P-1 23.211 Nil 0.046 0.303 0.817 2.828 3.186 4.931 6.705 2.642 0.203 1.55

T.P-2 20.95 Nil Nil 0.47 2.285 5.142 3.981 2.434 2.622 2.935 0.325 0.756

T.P-3 24.115 Nil 0.098 0.247 0.451 3.284 5.86 7.075 6.477 0.573 0.02 0.03

T.P-4 19.069 Nil 0.154 0.585 1.064 3.433 4.465 4.75 3.596 0.77 0.072 0.18

T.P-5 20.086 Nil Nil 0.103 0.557 2.191 2.906 3.929 7.01 2.983 0.308 0.099

T.P-6 22.559 Nil 0.223 0.756 1.27 3.215 4.578 5.494 6.751 0.24 0.02 0.012

T.P-7 20.33 Nil Nil 0.147 0.725 4.339 5.494 4.84 4.273 0.512 Nil Nil

T.P-8 23.748 Nil 0.416 0.529 1.776 6.332 7.728 4.821 2.142 0.004 Nil Nil

T.P-9 18.38 0.447 0.727 0.791 0.957 1.509 2.598 3.404 7.031 0.916 Nil Nil

T.P-10 16.73 Nil Nil 0.252 1.033 1.81 2.005 3.818 5.889 1.897 0.013 0.013

T.P-11 21.587 Nil Nil 0.356 1.263 4.526 2.462 5.013 6.228 1.373 0.301 0.065

T.P-12 20.835 0.126 Nil 0.165 1.648 5.183 3.486 4.194 5.192 0.841 Nil Nil

T.P-13 22.252 Nil 0.612 0.647 2.615 3.456 5.113 2.644 6.034 0.605 0.361 0.165

T.P-14 22.991 Nil Nil 0.458 2.489 6.874 2.469 3.754 4.586 1.691 0.586 0.084

T.P-15 19.525 Nil 0.542 0.648 1.64 4.157 3.009 2.648 6.338 0.543 Nil Nil

43

3.5 XRD of Ancient samples

3.5.1 Nagannathaswamy Temple

In the present research, the proportions of binder and aggregate were examined based on XRD

pattern.XRD analysis is very useful technique to identify the CaCO3 polymorphs (calcite,

aragonite and vaterite) for the investigation of the carbonation reaction of limeOur

interpretation is based on the assumption that the aggregate proportion corresponds to the

quartz and the binder to the calcite percentage. This assumption was derived from the earlier

petrographic study, which demonstrated a granitic origin of the aggregate and showed the

presence of calcite only as binder. As XRD can neither distinguish between carbonates in the

aggregate and in the lime paste coming from the binder nor amorphous phase like calcium

silica gel, the only detection noticed are crystalline phase resulting for carbonation and

hardening. In the present work semi quantification obtained through XRD gave an idea about

aggregate/binder proportions

Fig.20 XRD of Ancient Samples

44

Table 14 Minerals present in the XRD of Samples

Sample

s

Calcit

e

Ca

O

Quart

z

M

g

C

H

NS-1 ++ + +++ + +

NS -2 ++ +++ + - -

NS -3 +++ ++ + - +

From the XRD results of NS-1 it is observed that the main component of the plaster is Quartz, calcite

that is present abundant and other components such as calcium oxide, magnesium and CH are in very

less quantity. From the sample NS-2 it is observed that calcium oxide is present abundant and calcite is

in moderate range. The optical microscopy on the thin section of the plaster sample gave further

information about the binder, the type and shape of the aggregate materials and structure of the entire

components. The major minerals noticed in the plaster of NS-3 are calcite along with minor minerals

such as Calcium oxide and quartz. The results are in complete agreement with XRD data. Hence, the

high intense peaks observed in XRD(Fig 20 and Table 14) also indicates the pozzolanic reaction due to

addition of shell lime during burning, followed by hot lime technology and subsequent grinding of the

mortar mix. However, peaks indicate the formation of degradation products such as syngenite (K2Ca

(SO4)2.2H2O), gypsum (CaSO4) along with major calcite peaks throughout the range.

3.5.1 THANJAYUR PALACE

The XRD graph of TP-1, TP-2 and TP-3isshown in Fig 21. All the peaks are calcite except a

major sharp peak which indicates the presence of CSH and CAH phases in complex form of

gyrolite, stilbite and nechelyustovite.Stilbite (calcium sodium aluminium hydrate) belongs to

zeolite groups that are formed in the presence of sodium and calcium. Complex of CSH and

CAH is seen SEM images (Fig 5.7) indicating the hydro thermal products in flattened plate

crystals along with aggregates. Nechelyustovite is the hydrated phase of magnesium

oxide.These reaction phases are hydro thermal in nature, as shell lime with high percentage of

clay mineral would have been fired and slaked in hot water and allowed to mature for 1 to 3

months (Maroti and Kalmar 2006). This will result in micronisation of lime particles and make

it workable and reactive. After laying the mortar, simultaneously both hydration (hardening

45

under water) and carbonation (hardening by carbon- di – oxide) will take place. As the high

amount of carbon-di-oxide is available within the mortar due to fermentation of organics, more

calcite was formed. The presence of organics favoured the hydraulic reaction leading to the

initial formation of CSH and CASH. As the time progresses, all complex formation of CAH

and CSH will slowly re-carbonate into calcite. The results of XRD are confirmed with FT-IR,

TGA and DTA. In FT-IR (Fig 5.3) shows the wave band corresponding to 712, 874,

1440,1790,2515 and 2854 cm-1 of all samples of the temple indicate the formation of calcium

carbonate and co-existence of a small peak around 3430 cm-1 due to portlandite which was not

traced in XRD graphs.

Fig.21 Presence of possible minerals in mortars of Padaleeswarar temple

46

3.6 FT-IR of ancient samples

3.6.1 Nagannathaswamy Temple

Fig. 22 FT-IR of Ancient Samples

The samples of plasters and aggregates were examined under infrared spectroscopy (IR) the

analytical investigation was mainly carried to gather qualitative information about the major

components present in the plaster. The FTIR spectra were recorded in the region of 3500–500

cm_1 under a spectral resolution of 2 cm_1 for the powdered plaster samples. The aggregates

sieved after the digestion of plaster samples in dilute hydrochloric acid were also subjected to

similar examination.

A data for the FTIR spectra with spectra for inorganic and organic materials was used to

characterize the unknown materials present in the plaster. The characteristic peaks at

3427.11cm_1, 2511.90cm_1, 1794.24cm_1, 874.40cm_1, 715.68cm_1 were noticed to be calcite

and the peak at 1036.20 were observes to be aluminum silicates in the sample TS-1 of lime

mortar. The characteristic peak at 2513.35cm_1, 1795.09cm_1, 874.44cm_1, 715.64cm_1

47

arecalcite and were as peak 1631.45 is under group of CSH, the peak 1025.75cm_1 and 477.57

cm_1 were observed as silica and peak at 3442.84cm_1 confirmed the presence of protein in the

sample NS-2. The peak at 2514.47cm_1, 1796.47cm_1, 874.06cm_1, 712.79cm_1 were observed

to be the presence of calcite and the peaks at 476.77 and 460.12cm_1 are the compounds of

silica groups, 778.80cm_1 were observed to be quartz and 2924.28cm_1 were CH-bond

stretching groups of organics in the sampleNS-3. In support to organic analysis the peaks

3427.11cm_1, and 3431.88cm_1 in FT-IR corresponds to organics. The peak 3442cm_1 is found

to be portlandite. Peak 1033cm_1 is possibility of CSH,The peak indicates the presence of

amides (proteins) whereas 2924.28cm_1and indicates carbohydrates or polysaccharides. In

confirmation with organic test and FT-IR of samples indicates the presence of the organic

matter. It has been observed from the investigation of many of the Indian plasters that the

binding calcite is finally crystallized and surrounds the aggregate grains and partly fills the void

between the grains. Further, presence of finally crystallized calcite shows the almost total

conversion of Calcium hydroxide into Calcium carbonate by atmospheric Carbon dioxide in all

the plaster works, which is also the main reason for good tensile strength of those plasters,

which have no external contamination.

Additives were found to have transformed into calcium oxalate, revealed through FTIR

spectrum. Further, organic fibers and seeds were admixed to improve tensile strength and

reduce cracking in most plasters. From the results shown in figure5.5mixed with vegetal fibers

and seeds (high CO2 content) had been added to the plaster of along with lime .The proteic

materials and lime together have enhanced the binding properties of the earthen plaster.

3.6.2 THANJAVUR PALACE

As there are no vibrations corresponding to1420, 1450-1478 cm-1 and 1480 cm-1, there is no

possibility of formation of magnesite or hydromagnesite. However, in XRD, formation of

nechelyustovite may be due a small amount of MgO. A special band at 783 cm-1 in all the

samples infers the formation of calcite by biological growth that implies that microbial

carbonation of lime mortar has taken place(Fig 23).

48

Fig.23 FT-IR analysis of historic mortar at Thanjayur palace

3.7 Thermo gravimetric Analysis Results

3.7.1 Naganathaswamy temple

TG and DSC ( Fig 24 to 26) of sampleNS-1 curve of common lime mortar showed that

there were two obvious weight loss processes which belong to the decomposition of Ca (OH)2

and CaCO3, respectively. The broad endothermic decomposition 650.0 to 780.0 characterizes

amorphousand crystalline solids from CaCO3 calcite. The region bit 20 to 330 corresponding to

loss of absorbed water and dehydration of C-S-H phase.The DSC of ancient mortar showed that

there is a weight loss process, which belongs to the decomposition of calcium carbonate

temperature range of calcium carbonate from the peak of 650.0 to 780.0. Italso reveals

complete transformation of calcite from complex forms of CSH. The CSH gel can be stable in

natural form of gyrolite and okenite.Hence, the high intense peaks of CSH and CAH observed

in XRD also indicates the pozzolanic reaction due to addition of shell lime during burning,

followed by hot lime technology and subsequent grinding of the mortar mix. All carbonation

peaks are endothermic and around 730°c in these samples two types of reactions is done

49

hydration and carbonation. Exothermic peaks between 200 to 400 which indicates the presence

of organics

Fig.24 TGA Graph of NS-1

Fig.25 TGA Graph of NS-1

50

Fig. 26 TG-DSC Graph of NS-1

Fig.27 TG-DTG Graph of NS-2

51

Fig.28 TGA Graph of NS-2

Fig. 29 TG-DSC Graph of NS- 2

From sample TN-2 it is observed that the portlandite CSH, CAH and MgO is observed

more.The presence of organic admixtures enhances the formation of CSH, and CAH.The board

endothermic decomposition in the region of 650.0 to 780.0 characteristic of amorphous and

crystalline form of Caco3 and calcite. The region bit 20 to 330 corresponding to loss of

absorbed water ad dehydration of C-S-H phase. Hence in confirmation with XRD, the TGA

52

results indicates the shell lime rich in clay impurities along with limestone dehydroxylate

during burning process and acts as a pozzolan imparting early strength to the mortar. Also, the

dehydration of magnesia between 250 °C and 550 °C is seen in all the mortar samples that

substantially contribute to desirable plasticity. It is found that the co-existence of amorphous

and crystalline calcite enhances the hydration process as more amounts of free lime has been

available for reaction. As the age processes the complex forms of CAH and CSH phases re-

carbonate and forms CaCO3. Early decomposition of CaCO3 to CO2 between 600 °C and 770

°C and the major weight loss in this range shows that the hydraulic components (CSH like

gyrolite and okenite and CAH are completely transformed into CaCO3.

Fig.30 TG-DTG Graph of NS-3

53

Fig.31 TGA Graph of NS-3

Fig.32 TG-DSC Graph of NS-3

TG-DSC curves of ancient mortar displayed another weight loss process temperature ranges

from 120-400°c. This could be associated with the decomposition of organic in lime mortar.It

also reveals complete transformation of calcite from complex forms of CSH. TGA (Table 15)

data indicates the major weight loss in the range of 600–800 °C and it is due to decomposition

of calcite and release of CO2. It is definitely hydraulic in nature due to higher reaction of

carbonation. When heated up to 120 °C, the mortar containing less than or equal to 2% of

54

absorbed water demonstrate the absence of hygroscopic character, indicating lesser amount of

portlandite.

Table 15: Results of Thermal Analysis (Naganathaswamytemple )

Sample

Weight loss over temperature range (%) Structurally

bound

water %

CO2 /

H2O Total

weight

Loss

(%)

Inference

< 120

° C

120 -

400°C

400 -

550°C

600-

800

° C

800-

1000°

C

NS -1 0.55 0.88 0.55 9.03 0.2 1.43 6.31 11.21 New

mortar

NS -2 3.48 5.54 2.8 8.42 1.61 9.04 0.93 20.24 Old

mortar

NS -3 0.78 3.72 2.29 16.89 - 4.5 3.75 23.68 Old

mortar

3.7.2 TGA at Thanjavur palace

TGA is in agreement with XRD. In the analysis of weight loss based on TGA results (Table

16), four ranges of temperature are considered. In the range of 0 to 120°C, the weight loss

percentage of TP-1, TP-2 and TP-3 samples are 0.125, 0.41 and 0.67, respectively. In this

range, weight loss is associated with hygroscopic water.As percentage is very less for both

exterior walls TP-1andTP-2 indicating that they are totally carbonated compared to inner wall

TP-3 whichhas more water content. In the temperature range 200oC – 650°C weight loss is

because of structural bound water which is due to dehydration of hydraulic compound.

Structural bound water of all the samples were in the range of 5 – 14 % that implies that natural

pozzolans have been added to the mortars. As observed by Moropoulou et al (1995) and

Moropoulou et al (2000) the percentage of CO2 due to decomposition in the range of 600oC -

800° C is in the range of 12-20.The value of CO2 / H2O which inversely expresses the level of

hydraulicity is less than 3, hence the mortars are hydraulic in nature. The hydraulic mortars

with high clay as pozzolanic materials were used as a binder and the high level of CO2 in

mortars as possible because of the addition of cocktail of herbs added to improve the properties

of mortar.

55

Table 16: Results of Thermal Analysis(Thanjavur Palace)

Sample

Weight loss per temperature Range (%)

< 120 ° C 120 -400°C 400 -550°C 600 - 800° C

TP-1 0.125 0.48 0.55 16.73

TP-2 0.41 1.02 0.70 11.01

TP-3 0.67 0.53 0.53 11.04

In DTA analysis of samples TP-1, TP-2andTP-3 shows a very narrow endothermic peak near

868.9oC, 806.6°C and 823°C, respectively. This is due to the formation of calcite in the

recarbontion zone of 800o-900°C. The CSH and CASH are initially formed due to hydration

and after long exposure to carbon-di-oxide, it will further completely transformed into calcite.

The formation of more amounts of CSH and CASH is due to presence of the clay minerals.

Elsen (2006) has expressed that there is a traditional practice of using the clay minerals fired at

600° C to 900°C to gain a distinct pozzolanic activity in India or lime with high clay minerals

is used. The clay minerals are nano materials whose particle size is less than 2 µm. Because of

thetiny size of the particle, clay minerals have a larger surface area with string electrostatic

interactions (Singh and Arbad 2014).

The fired clay minerals are alumina silicate with rich calcium content which will act as zeolites.

This improves the workability and reduces chlorine permeability is much suitable for the

marine environment. This proves the main aim of our ancestors to produce hydrated phases

similar to natural minerals and had reqiured properties like strength and long term stability

(Stefanidouet al 2013). Similarly in all samples the exothermic reaction in the range of 300oC

to 400°C infers that organics is added to the mortar. They may be rich in carbohydrate as the

TGA indicated a high level of CO2. In Tamil Nadu, fermented jaggery and kadukai juice are

added in lime mortar construction. For the weatherproof course for houses, addition of surthi,

limestone, shell lime along with jaggery and kadukai extract is still prevalent in south India.

Borges et al(2014) has discussed that the recarbonation of CSH and CAH is only possible in

hydraulic lime mortars. As the recrystallisation of calcium carbonate takes place, the crystals

56

formed will occupy the pores that will contribute to the compactness of the mortar matrix by

fulfilling the porous structure.

The exothermic peaks near 400°C in all samples show the decomposition of organic matter or

aluminium hydroxides. The endothermic peaks of 571.8, 574.1 and 571.6°C for TP-1, TP-

2andTP-3, respectively show the presence of quartz phase change. In all the samples, the peaks

62.3, 106.1 and 74.1° C show the dehydration of CSH and CAH confirms the hydraulic

character of lime. (Mertenset al2009). Figures 33,34 and36 show TGA and DTA of samples

TP-1, TP-2 and TP-3, respectively.

Fig.33 TGA and DTA of TP-1Samples

57

Fig. 34 TGA and DTA of TP-2 Sample

Fig.35 TGA and DTA of TTP-3 Sample

58

3.8 SEM INTERPRETATION

3.8.1 Naganathaswamy Temple

SEM images are presented from Fig.36 to 38. The images clearly support the other analytical

techniques and shows the formation of calcite crystals. The amorphous form of calcite is also

present.The lime sand matrix is very compact in all the images. The complete carbonation on

external surface is evident. The presence of organics is confirmed by simultaneous presence of

amorphous and crystal calcite.

Fig. 36 Lime sand matrix

59

Fig. 37 Compact strutures of lime mortar

Fig. 38 Crystal forms of calcite

3.8.2 SEM images at Thanjavur palace

In SEM images as represented in Fig. 39, aragonite fibrous form of calcite develops ring

texture around sand grains. The big grains show calcium silicate hydrate (CSH), which is the

prime ingredient in hardening hydraulic lime. Aragonite is formed due to addition of clay

60

minerals at higher temperature similar to the presence of zeolites (Andrejkovicaetet.al 2012).

They are seen along the long voids as in Fig 40. The Fig. 41 shows the formation of calcite

crystals. Further there is a formation of nano clusters of calcite which are polydispersed and

compact. They have specific crystallographic orientation that contributes to an agglomeration

process. The Fig. 42 shows the white layer heaped on the top of sand grain and rhombohydral

forms of calite in Figure 43.There are no cracks in the mortar sample on further magnification.

As the mortar is in good condition still after many centuries exposed to the marine environment

may be due to the presence of organic matter that acts as an inhibitor to crystallization.

Fig. 39 Aragonite formation of calcium carbonate

61

Fig. 40 Long voids in between the mortar

Fig. 41 Calcite crystals

62

Fig. 42 White layers heaped on the top of sand grain

Fig.43 Formation of rhomhedral crystals of calcite

63

3.9 NEW MORTAR SIMULATION

3.9.1 Characteristics of lime

Chemical characteristics of lime such as oxides of calcium and magnesium, silica, alumina and

iron are determined, and their significance on the behavior of lime are discussed to ascertain

the class and hydraulicity of lime. Field tests are conducted on lime, and the observations are

correlated to classify the lime. Influence of admixtures on the setting time of lime is also

discussed in this section.

3.9.2 Chemical characteristics of lime

The results of chemical composition of lime determined as per IS: 6932 (Part V) - 1973 are

given in Table 17. Total binder content (calcium and magnesium oxides) is 64.6 %, which is

greater than the minimum requirement of 60% for Class A structural lime as per Indian

Standards, IS: 712 - 1984. Total clay content (silica, alumina and ferric oxide) is equal to

28.33% which is greater than the minimum requirement of 10% for Class A lime as per

IS: 712 - 1984. From the results the lime can be classified as class A lime that could be used for

the construction of structural elements.

Table 17 Chemical composition of lime

Sl.

No. Chemicals

Composition

(%)

Limits as per IS: 712-1984

for Class A Lime

1. Calcium and magnesium oxides

(on ignited basis)

64.90 60 % minimum

2. Magnesium oxides

(on ignited basis)

1.21 6 % maximum

3. Silica, alumina and ferric

oxides.(on ignited basis)

28.33 10 % minimum

4. Ferric oxides 2.29 -

5. Unhydrated magnesium oxide Nil -

6. Insoluble residue in dilute acid

and alkali (on ignited basis)

12.90 15% maximum

- Limits are not specified in IS 712-1984

64

3.10 HYDRAULICITY OF LIME

Hydraulic Index (HI) is an indication of the hydraulicity of lime. It is based on the oxides

content in lime. Hydraulic index of the lime used in the study is equal to 0.43. Eminently

hydraulic lime have values greater than 0.4 (Cowper 2000).Hence, the lime used is categorized

as eminently hydraulic.

3.11 FIELD TESTS ON LIME

The outcome of the field tests conducted as per IS: 1624 - 1986 are presented in Table 18. The

inferences are discussed to assess the nature of lime. Lime is examined visually for the colour,

texture, fineness and the presence of grit particles. On visual examination, the lime used for the

investigation is light grey and does not contain coarse and gritty lime pieces larger than 2.30

mm. Hence, it could be categorized as Class A lime.

In the hydrochloric acid test, a thick gel formation is observed and did not flow out of the glass

tube when tilted, which shows signs of Class A Lime.

Results of the ball test infer that there are no signs of disintegration after six hours observation

of the prepared lime ball (50 mm diameter). Hence, the lime is categorized as Class A,

structural lime.

Table 18 Field tests on lime

Test

Conducted Observation Inference

Visual

examination

Does not contain coarse and gritty lime pieces

larger than about 2.30 mm

Class A, structural lime

Ball test Sign of disintegration in the ball of 50mm

diameter after six hours

Class A, structural lime

Hydrochloric

acid Test

A thick gel formation observed and did not

flow out of the cylinder when tilted

Class A, structural lime

65

Table 19 Sample Description

Category Description

Category 1 12.5% of jaggery and 2.5 of kadukkai

Category 2 12.5 of kadukkai and 2.5 of jaggery

Category 3 6.25 % jaggery and 6.25 % of kadukkai

3.12 TEST RESULTS OF CONSISTENCY AND SETTING TIME OF LIME

The results of consistency and setting time of reference lime and admixture-modified lime are

presented in Table 20. It was observed that the consistency of admixtures lime mortar of

categories1, 2,3 gradually increases with the reference.The initial and final setting time of lime

was found to be increased in admixture lime in comparison to the reference lime mortar.

1st category is of 12.5% of jaggery and 2.5 of kadukkai, 2nd category of 12.5 of kadukkai and

2.5 of jaggery and 3rd category is of combinations of both category of percentage 12.5%.

Table 20 Consistency and Setting Time of Lime

Category Consistency (%) Initial setting time

(In minute)

Final setting time

(In minute)

Reference 64% 300 900

1 70% 330 1500

2 69% 430 1430

3 70% 410 1400

3.13TEST RESULTS ON COMPRESSIVE STRENGTH OF HYDRAULIC LIME MORTAR

The compressive strength of hydraulic lime mortar of admixture modified was comparatively

lower and more or less equal to the normal conventional lime mortar. Though the compressive

strength of admixture modified lime mortar is low it had a good flexural strength.

66

Table 21 Compressive strength of hydraulic lime

Sample Compressive Strength in MPa

28 Days 90 Days

Reference 1.52 2.70

HL1 1.01 1.85

HL2 1.87 2.52

HL3 1.95 2.67

3.14 Test results on Compressive strength of Air lime mortar

The results of compressive strength of Air lime mortar and admixture modified at 28, and 90

days are presented in Table 22. The compressive strength of Air lime mortar of admixture

modified was comparatively higher than the normal conventional lime mortar. The strength

gradually increases with the category 1,2 and 3. The category 3 has an increasing compressive

strength of 53% than the reference lime mortar.

Table 22 Compressive strength of Air lime

Sample Compressive Strength in MPa

28 Days 90 Days

Reference 1.38 2.10

AL1 1.19 1.63

AL2 1.58 2.45

AL3 2.56 3.21

67

Fig. 44 Mode of failure of cube specimen

5.10.4 Test results on Flexural Strength of hydraulic lime mortar

Table 23 Flexural Strength of Hydraulic Lime

Sample Flexural Strength in MPa

28 Days 90 Days

Reference 0.48 1.98

HL1 0.56 2.51

HL2 0.45 1.68

HL3 0.39 0.78

It is observed that good increase in Flexural strength of admixture modified lime mortar than

the conventional lime mortar. The flexural strength of category 1 added lime mortar had a peak

value of 2.51 N/mm2 at 90th day and 0.56N/mm2 at 28th day. The category 1 has an increasing

flexural strength of 60% to the reference mortar. Then the flexure strength gradually decreases

with category 2 and 3.

68

5.10.5 Test results on Flexural Strength of Air lime mortar

Table 24 Flexural strength of Air lime

Sample Flexural Strength in MPa

28 Days 90 Days

Reference 0.22 0.12

AL1 0.45 0.18

AL2 0.34 0.56

AL3 0.60 0.16

The results of flexure strength of the air lime mortar on reference lime concrete and admixture

modified concrete at 28 and 90 days are presented in Table 24. The flexure strength of concrete

was found to be increased gradually of 64%at 28 days in three categories than the reference

mortar. Lime with admixtures dosage increases the flexural strength of the mortar with age, in

comparatively with the reference mortar.

Fig.45 Mode of failure of prism specimen

69

5.10.6 Water Retentivity test

The percentage of water retended in the admixture modified lime mortar varies for every 5min.

Since the admixture modified lime mortar had a good water retentive capacity it will have low

shrinkage, good workability and also it enhance the hydration process. The water retention

capacity of various proportions of admixtures modified lime mortar is expressed in percentage

and is given in the Fig.46, 47 and 48.

Fig.46 Water Retentivity test Results of category No.1(HL1)

Fig. 47 Water Retentivity test Results of category No.2(HL2)

WA

TER

REN

TEN

TIV

TY(%

)

TIME (IN MIN)

Wat

er

Re

nte

ntv

ity

(%)

TIME (in min)

70

Fig. 48 Water Retentivity test Results of category No.3 (HL3)

5.10.7 PHYSICAL PROPERTIES

The bulk density of admixture modified lime mortar was gradually increasing and

hence there is an increase in unit mass. The percentage of water absorption and porosity

decreases gradually for increasing percentage of admixtures with water. Since there was a

decrease in percentage of water absorption and porosity it enhances the durability

characteristics and also resist the rainwater penetration.

Table 25 Physical properties of hydraulic lime

Sample Bulk density

(g/cm3)

Water

absorption (%)

Porosity

(%)

Capillary

absorption

1 1.568 19.38 30.40 1.4x10-3

2 1.736 10.40 18.05 1.5x10-3

3 1.775 11.12 19.54 1.6x10-3

WA

TER

RET

ENTI

VIT

Y(%

)

TIME (IN MINUTES)

71

Table 26 Physical properties of Air lime

Sample Bulk density

(g/cm3)

Water

absorption (%)

Porosity

(%)

Capillary

absorption

Reference 1.692 19.38 21.53 1.8x10-3

1 1.696 12.5 21.12 1.6x10-3

2 1.765 6.194 10.93 1.5x10-3

3 1.693 10.47 17.74 1.3x10-3

72

Chapter 4

CONCLUSIONS

The properties of characterized and simulated mortars required for Naganathasamy Temple and

Thanjavur Palace is summarized in Table 27.

Table 27 Properties of characterized and simulated mortars

Description

Naganathaswamy Temple Thanjavur Palace

Characterization

study

Simulated

mortar

Characterization

study

Simulated mortar

B/A ratio 1: 3 to 1: 7 1: 3 1: 3 to 1: 6 1: 3

Lime mortar

classification Hydraulic lime Limestone

( HL)

Hydraulic lime

with artificial

pozzolans

Lime stone ( HL)

Organic

materials

Carbohydrates

and proteins

6.25 %

Kadukai and

6.25% Jaggery

Carbohydrates

and proteins

12.5 %Kadukai and

2.5% Jaggery with

brick dust

Compressive

strength(N/mm2) 3-5 2.66 1.37-4.60 1.8

Flexural

strength

(N/mm2)

Less than 0.5 0.394 0.5-1.0 0.563

Bulk density

(g/cm3)

1.7-2.1 1.7 1.5-1.9 1.56

Porosity

(%) 18-20 19.54 40 30.4

73

Based on the study output the restoration of the both structures can be carried out. The results

of the experimental investigation will be much helpful for the Department of Archaeology both

for conservation of the ancient monuments and for preparation of restoration mortars which

will make our Country’s Monuments to stand rigid for further centuries.

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