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Development of Unfired Bricks using Industrial Waste

Thesis · July 2016

DOI: 10.13140/RG.2.2.23905.51047

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 DEVELOPMENT OF UNFIRED BRICKS USING
INDUSTRIAL WASTE

By
SANDEEP JAIN
(2014CET2226)

Submitted in partial fulfilment of the requirement for the award of degree of

MASTER OF TECHNOLOGY
In
CONSTRUCTION ENGINEERING AND MANAGEMENT

Under the guidance of

Dr SHASHANK BISHNOI

To the
DEPARTMENT OF CIVIL ENGINEERING
INDIAN INSTITUTE OF TECHNOLOGY DELHI
JUNE 2016
 ACKNOWLEDGEMENT
Though only my name appears on the cover of this report, a great many people have contributed
to its production. I owe my gratitude to all those people who have made this report possible
and because of whom my project experience has been one that I will cherish forever.
My deepest gratitude is to my advisor, Dr Shashank Bishnoi, Department of Civil
Engineering. I have been amazingly fortunate to have an advisor who gave me the freedom to
explore on my own, and at the same time the guidance to recover when my steps faltered. His
vast knowledge and constant encouragement helped me during all the stages of this work and
also in preparation of this report.
I would like to thank Dr B. Bhattacharjee, Dr Uma Maheswari (program coordinator), and Dr
K. C. Iyer (DRC nominee) who through their valuable suggestions and continuous
encouragement guidance.
I am also grateful to Mr Vinit Shah for his practical advice and encouragement. I am also
thankful to him for commenting on my views and helping me understand and enrich my ideas.
I would also like to thank Mr Vinish, Manoj, and Krishna (laboratory staff) who helped me to
carry out different experiments and casting in the laboratory.
Special appreciation goes to all my friends at the institute and colleagues from the Materials
Research Laboratory for their friendship and the dynamic atmosphere.
At this occasion, I would also like to convey my gratitude to Mr Soumen Maity for having
provided necessary inputs at different stages of the project.
I would like to express my gratitude to my family for all the love and support they extended.
Finally, I am grateful to the almighty for his grace to carry out my study.
Date: 01/07/2016
Sandeep Jain
(2014CET2226)

i
 ABSTRACT
India, being the fastest growing economy in the world, is currently on the verge of large scale
urbanisation hence facing a huge demand for building houses and so the materials to build
them. To cope up with this housing necessity, the country needs to build 30 to 35 thousand
units of houses per day at least for the next 8 years. The shelter is the primary need of every
human being. As for the human body, carbons are the building block, bricks are the building
blocks of a house. India being the second largest producer of bricks after China, produces 236
billion bricks per year consuming a huge amount of natural resources like soil, sand, coal, etc.
Conventional red bricks are commonly made from a mixture of clay and sand, moulded to a
rectangular shape, dried off and then burned into a kiln at a high temperature of 900 to 1200°C.
India's brick industry, spread out over 100,000 kilns, is a big source of pollution. To fire bricks
to hot temperatures, the kilns uses huge amounts of coal and diesel, and the residue is
horrendous: thick particulate matter, poor working conditions, and lots of climate-changing
emissions. To overcome the issues related to conventional bricks, utilization of various
industrial waste material in brick making has gained much popularity in India and a many of
these industrial waste has been tried out successfully to produce bricks. But one major issue
for their commercial production is that there is no such standardised process or methodology
available for them like we have for the production of concrete, except for ‘fly ash-sand-lime-
gypsum’ system which people have developed through experimentation over a long period of
time based on trial and error approach.
This project aims to develop unfired, non-structural, binder brick with 100% waste material
using fly ash, pond ash, and local industrial waste like coal cinder, paper sludge, and marble
dust with lime and gypsum system to alleviate resources like coal and diesel, preservation of
top soil, prevention of harmful emissions and managing the industrial waste. This study is
primarily focused on optimization of the compressive strength of newly developed bricks,
while minimizing weight density, and water absorption, through extensive laboratory work.
The ultimate objective of undertaking this topic as a project work is to identify variables
affecting the various properties of bricks. On successful completion of this study, this
methodology shall enable us to consciously produce bricks out of industrial waste based on the
characterization, packing, and other engineering properties.
Key Words: Unfired bricks, fly ash bricks, pond ash bricks, coal cinder bricks, paper sludge
bricks, marble dust brick, packing density, ultrasonic pulse velocity (UPV), and initial porosity

ii
 TABLE OF CONTENTS

ACKNOWLEDGEMENT .......................................................................................................... i

ABSTRACT ...............................................................................................................................ii

TABLE OF CONTENTS ......................................................................................................... iii

LIST OF FIGURES .................................................................................................................. vi

LIST OF TABLES ................................................................................................................. viii

CHAPTER 1: INTRODUCTION .............................................................................................. 1

1.1 General ............................................................................................................................. 1

1.2 Present scenario and need for research ............................................................................ 1

1.3 Research objectives .......................................................................................................... 5

1.4 Scope of work .................................................................................................................. 6

1.5 Organisation of the thesis................................................................................................. 6

CHAPTER 2: LITERATURE REVIEW ................................................................................... 7

2.1 General ............................................................................................................................. 7

2.2 Production of conventional bricks ................................................................................... 7

2.3 Fly ash bricks ................................................................................................................... 9

2.4 Optimization of process parameters............................................................................... 10

2.5 Effect of utilization of various industrial waste in bricks .............................................. 10

CHAPTER 3: MATERIALS ................................................................................................... 14

3.1 General ........................................................................................................................... 14

3.2 Fly ash ............................................................................................................................ 14

3.3 Pond ash ......................................................................................................................... 15

3.4 Stone dust ....................................................................................................................... 16

3.5 Coal cinder ..................................................................................................................... 16

3.6 Paper sludge ................................................................................................................... 17

3.7 Marble dust .................................................................................................................... 17

3.8 Quicklime....................................................................................................................... 18

iii
 3.9 Gypsum .......................................................................................................................... 18

CHAPTER 4: EXPERIMENTS ............................................................................................... 19

4.1 Research methodology ................................................................................................... 19

4.2 Raw material characterization........................................................................................ 20

4.2.1 Specific gravity test................................................................................................. 20

4.2.2 Loss on ignition....................................................................................................... 21

4.2.3 Water absorption test .............................................................................................. 22

4.2.4 Blaine’s fineness test............................................................................................... 23

4.2.5 Image Analysis........................................................................................................ 24

4.2.6 X-ray powder diffraction (XRD) ............................................................................ 25

4.3 Reactivity of raw materials ............................................................................................ 30

4.3.1 Lime Reactivity....................................................................................................... 30

4.3.2 Isothermal calorimetry ............................................................................................ 31

4.4 Casting of specimens ..................................................................................................... 32

4.4.1 Mixture proportioning of specimens ....................................................................... 32

4.4.2 Casting methodology .............................................................................................. 34

CHAPTER 5: RESULTS & DISCUSSION ............................................................................ 36

5.1 Results ............................................................................................................................ 36

5.1.1 Compressive strength test ....................................................................................... 36

5.1.2 Ultrasonic pulse velocity test (UPV) ...................................................................... 37

5.1.3 Water absorption & bulk density test...................................................................... 39

5.1.4 Efflorescence test .................................................................................................... 41

5.1.5 Initial porosity ......................................................................................................... 41

5.2 Discussion ...................................................................................................................... 43

5.2.1 Compressive strength test ....................................................................................... 43

5.2.2 Relationship between ultrasonic pulse velocity, compressive strength, density and
water absorption ............................................................................................................... 46

iv
 5.2.3 Effect of industrial waste on water absorption and bulk density ............................ 50

5.2.4 Efflorescence........................................................................................................... 52

5.2.5 Effect of initial porosity on compressive strength, UPV, water absorption and bulk
density .............................................................................................................................. 53

CHAPTER 6: SUMMARY & CONCLUSIONS .................................................................... 56

6.1 Summary ........................................................................................................................ 56

6.2 Conclusions .................................................................................................................... 57

6.3 Future perspectives ........................................................................................................ 59

REFERENCES ........................................................................................................................ 60

v
 LIST OF FIGURES
Figure 1.1: World brick production (Source: Eco Brick) .......................................................... 1
Figure 1.2: Conventional brick production - problem tree ........................................................ 3
Figure 1.3: Proposed brick production - objective tree.............................................................. 5
Figure 2.1: Strength development mechanism (Sintering) of conventional fired clay bricks ... 8
Figure 2.2: Cause-and-effect diagram for processing of fly ash brick .................................... 11
Figure 4.1: Raw material characterization ............................................................................... 19
Figure 4.2: Tests on brick specimens ....................................................................................... 19
Figure 4.3: 'Le chatelier' flask & Pycnometer bottle ............................................................... 20
Figure 4.4: Muffle Furnace ...................................................................................................... 21
Figure 4.5: Water absorption test ............................................................................................. 22
Figure 4.6: Blaine’s air permeability test apparatus ................................................................ 23
Figure 4.7: Image analysis {(a). Stone dust, (b). Pond ash, (c). Coal cinder, (d). Paper sludge}
.................................................................................................................................................. 25
Figure 4.8: XRD sample preparation & placement ................................................................. 26
Figure 4.9: X-Ray Diffractometer (Bookers XRD, D8-ADVANCE) ..................................... 27
Figure 4.10: XRD result for fly ash ......................................................................................... 27
Figure 4.11: XRD result for pond ash ...................................................................................... 27
Figure 4.12: XRD result for stone dust .................................................................................... 28
Figure 4.13: XRD result for marble dust ................................................................................. 28
Figure 4.14: XRD result for coal cinder .................................................................................. 28
Figure 4.15: XRD result for Paper Sludge ............................................................................... 29
Figure 4.16: XRD result for quicklime .................................................................................... 29
Figure 4.17: XRD result for gypsum ....................................................................................... 29
Figure 4.18: Flow table test for lime reactivity........................................................................ 30
Figure 4.19: Isothermal calorimetry results ............................................................................. 31
Figure 4.20: Casting of various brick specimens ..................................................................... 34
Figure 5.1: Compression testing machine ................................................................................ 36
Figure 5.2: UPV apparatus ....................................................................................................... 38
Figure 5.3: Compressive strength (MPa) for replacement of stone dust with pond ash in base
mix ........................................................................................................................................... 43
Figure 5.4: Compressive strength (MPa) for replacement of fly ash from reference mix with
pond ash and coal cinder at different curing age ..................................................................... 44

vi
Figure 5.5: Comparison of compressive strength (MPa) for replacement of fly ash with pond
ash and coal cinder in reference mix at curing age of 56 days ................................................ 44
Figure 5.6: Compressive strength (MPa) for addition of paper sludge and marble dust to the
reference mix at different curing age ....................................................................................... 45
Figure 5.7: Comparison of compressive strength (MPa) for addition of paper sludge and marble
dust to the reference mix at curing age of 28 days .................................................................. 46
Figure 5.8: UPV (km/s) for series A blends at different curing age ........................................ 46
Figure 5.9: UPV (km/s) for series B blends at different curing age ........................................ 47
Figure 5.10: UPV (km/s) for series C blends at different curing age ...................................... 48
Figure 5.11: UPV (km/s) for series D blends at different curing age ...................................... 48
Figure 5.12: UPV (km/s) for series E blends at different curing age ...................................... 48
Figure 5.13: Relationship between compressive strength (MPa) and UPV (km/s) at the age of
28 days ..................................................................................................................................... 49
Figure 5.14: Relationship between bulk density (g/cc) and UPV (km/s) at the age of 28 days
.................................................................................................................................................. 49
Figure 5.15: Relationship between water absorption (%) and UPV (km/s) at the age of 28 days
.................................................................................................................................................. 50
Figure 5.16: Relationship between compressive strength and average water absorption at the
age of 28 days .......................................................................................................................... 51
Figure 5.17: Relationship between average bulk density and compressive strength for various
blends of series, at the age of 28 days ...................................................................................... 52
Figure 5.18: Effect of initial porosity on compressive strength of bricks at the age of 28 days
.................................................................................................................................................. 53
Figure 5.19: Effect of initial porosity on UPV of bricks at the age of 28 days ....................... 54
Figure 5.20: Effect of initial porosity on water absorption of bricks at the age of 28 days ..... 54
Figure 5.21: Effect of initial porosity on bulk density of bricks at the age of 28 days ............ 54

vii
 LIST OF TABLES
Table 4.1: Specific gravity of raw materials ............................................................................ 21
Table 4.2: Loss on ignition (LOI) ............................................................................................ 22
Table 4.3: Water absorption of raw materials .......................................................................... 22
Table 4.4: Fineness (Blaine’s value) for raw materials ........................................................... 24
Table 4.5: Lime reactivity of raw materials ............................................................................. 30
Table 4.6: Blends for isothermal calorimetry .......................................................................... 31
Table 4.7: Blends for replacement of stone dust from base mix with pond ash ...................... 32
Table 4.8: Replacement of fly ash from reference mix with pond ash .................................... 33
Table 4.9: Replacement of fly ash from reference mix with coal cinder ................................. 33
Table 4.10: Addition of paper sludge to the reference mix ..................................................... 33
Table 4.11: Addition of marble dust to the reference mix ....................................................... 34
Table 5.1: Compressive strength (MPa) results at different ages for replacement of stone dust
from base mix with pond ash (Series A) .................................................................................. 36
Table 5.2: Compressive strength (MPa) results at different ages for replacement of fly ash from
reference mix with pond ash (Series B) ................................................................................... 37
Table 5.3: Compressive strength (MPa) results at different ages for replacement of fly ash from
reference mix with coal cinder (Series C)................................................................................ 37
Table 5.4: Compressive strength (MPa) results at different ages with addition of paper sludge
to the reference mix (Series D) ................................................................................................ 37
Table 5.5: Compressive strength (MPa) results at different ages with addition of marble dust to
the reference mix (Series E) ..................................................................................................... 37
Table 5.6: UPV (km/s) results at different ages for replacement of stone dust from base mix
with pond ash (Series A) .......................................................................................................... 38
Table 5.7: UPV (km/s) results at different ages for replacement of fly ash from reference mix
with pond ash (Series B) .......................................................................................................... 38
Table 5.8: UPV (km/s) results at different ages for replacement of fly ash from reference mix
with coal cinder (Series C) ....................................................................................................... 39
Table 5.9: UPV (km/s) results at different ages for addition of paper sludge to the reference
mix (Series D) .......................................................................................................................... 39
Table 5.10: UPV (km/s) results at different ages for addition of marble dust to the reference
mix (Series E) .......................................................................................................................... 39

viii
Table 5.11: Average water absorption (%) and bulk density results for replacement of stone
dust from base mix with pond ash (Series A) .......................................................................... 40
Table 5.12: Average water absorption (%) and bulk density results for replacement of fly ash
from reference mix with pond ash (Series B) .......................................................................... 40
Table 5.13: Average water absorption (%) and bulk density results for replacement of fly ash
from reference mix with coal cinder (Series C) ....................................................................... 40
Table 5.14: Average water absorption (%) and bulk density results for addition of paper sludge
to the reference mix (Series D) ................................................................................................ 40
Table 5.15: Average water absorption (%) and bulk density results for addition of marble dust
to the reference mix (Series E)................................................................................................. 41
Table 5.16: Initial porosity results for replacement of stone dust from base mix with pond ash
(Series A) ................................................................................................................................. 42
Table 5.17: Initial porosity results for replacement of fly ash from reference mix with pond ash
(Series B) ................................................................................................................................. 42
Table 5.18: Initial porosity results for replacement of fly ash from reference mix with coal
cinder (Series C) ...................................................................................................................... 42
Table 5.19: Initial porosity results for addition of paper sludge to the reference mix (Series D)
.................................................................................................................................................. 42
Table 5.20: Initial porosity results for addition of marble dust to the reference mix (Series E)
.................................................................................................................................................. 42
Table 6.1: Comparative compressive strength for various bricks blend used in this study ..... 59

ix
 CHAPTER 1: INTRODUCTION

1.1 General
India is the world’s fastest developing country with an economic growth rate averaging 7.5%
for last 5 years. We are currently on the verge of large-scale urbanisation hence facing a huge
demand for building houses and thus for the materials to build them. The construction industry
contributes to about 10% of Gross Domestic Production (GDP) of the nation, registering an
annual growth of about 9% (www.ecobrick.in 2015). To cope up with this housing necessity,
the country needs to build 30 to 35 thousand units of houses per day at least for the next 8
years. Housing is the primary need of every human being. As for the human body, carbons are
the building block, bricks are the building blocks of a house. Clay fired bricks form the
backbone of the construction industry, which is valued at approximately US$ 70.8 billion. The
brick making is a traditional but important industry in India and other developing nations. The
brick sector in India, although unorganised, is tremendous in size and spread with annual brick
production growth of 5 to 10%. India is the second largest brick producer in the world after
China as shown in Figure 1.1. India is estimated to have more than 1,45,000 registered and
unregistered brick-making enterprises producing more than 236 billion bricks and providing
direct employment to more than 8 million workers (Jain and Singh 2009). It is continually
expanding on account of a rapid increase in demand for bricks in infrastructure and housing
industry.

Others
23%

Bangladesh
4% China
54%
Pakistan
8%

India
11%

Figure 1.1: World brick production (Source: Eco Brick)

1.2 Present scenario and need for research

As per the report by Punjab State Council for Science and Technology (PSCST), the brick
technology in India varies from region to region and generally depends on the scale of
1
production, soil and fuel availability, demand, market conditions and also on the enforcement
of the law for shifting from one technology to the other. The brick production in India takes
place in units using century old production methods, involving manual and inefficient methods
of clay preparation, hand moulding, and firing. Since the drying and firing are done in open,
the brick cannot be dried and fired during the rainy season, hence is mostly seasonal and
operating from 6 to 8 months. 70% of brick production takes place in Indo-Gangetic plains
consisting of the north and north-eastern parts of India using Bull’s Trench Kiln (BTK)
technology with fixed chimney. In peninsular India, the majority of brick production is through
clamp kilns and BTKs. The main fuel used is coal and biomass (Jain and Singh 2009). Brick
making is a highly energy intensive process, with a specific energy consumption of 1.2 to 1.75
MJ/kg of fired bricks for Bull's trench kilns, and 1.5 to 3.0 MJ/kg of fired bricks for clamp kilns
(Maithel and Uma 2000).
Central Pollution Control Board (CPCB) has recognized the brick production industry as a high
resource and energy intensive and polluting industry owing to the prevalence of obsolete
production technologies. While, the clusters are the source of local air pollution affecting local
population, agriculture, and vegetation; at a global scale, they also contribute to climate change.
It poses a significant challenge to brick industry due to competition with other sectors for
resources. Coal and top soil are two such resources. Coal is required for the power, steel and
other crucial sectors and the top soil or land which could be used for agriculture. The traditional
kiln unit itself occupies a considerable land area and is subjected to high temperature, making
it unfit for agricultural activities (after the site is abandoned). The fast depletion of arable land
thus caused due to brick making is a matter of concern to India regarding food security. Brick
sector consumes about 27 million tonnes of coal per year, with an average consumption of
about 18 tonnes of coal per 100,000 units of bricks, which is 8% of the total coal consumption
of the country and the third largest consumer after power and steel sector. In addition to coal,
brick sector also consumes several million tonnes of biomass fuels (www.ecobrick.in 2015).
The approximate clay consumption of 500 million m3 is estimated annually (Komyotra 2005).
Low efficiency in brick firing practices leads to high levels of PIC (product of incomplete
combustion) emissions. The burning of coal for high temperature requirement in production of
conventional burnt bricks is also responsible for emissions of carbon dioxide (CO2), carbon
monoxide (CO), sulfur dioxide (SO2), nitrogen dioxide (NO2) and suspended particulate matter
(SPM) which causes considerable health problems, especially related to respiration while also
causing damages to properties and crops. It is estimated that about 66 million tonnes of carbon
dioxide (CO2) are emitted into the atmosphere due to brick production in India (Komyotra
2
2005). On one hand, conventional brick-making sector is facing issues of resource depletion in
terms of coal and top soil erosion along with other harmful emissions and particulate matter
making the brick production process unsustainable (Figure 1.2 shows problems caused by
conventional brick production and their effects). On the other hand, a huge amount of industrial
waste like fly ash, pond ash, coal cinder, paper sludge, rice husk ash, blast furnace slag, marble
dust etc. are waiting to be utilized as a resource. A lot of research is ongoing for possible
utilization of such waste that otherwise goes unmanaged or in landfills.

Socio-Economic Conditions

Scarcity of Landfill Sites

Loss of Agricultural Top-Soil

Effects
Effect on Building Industry & Environmental Damage, Carbon
economy, Higher End-Consumer Emission, Global Warming
Prices

Unsustainable Production & Process (Conventional Bricks) Problem

High Energy Consumption Environmental

through Intensive Firing Pollution
Causes

High Resource Increase in Industrial Waste

Consumption

Obsolete Technologies,
Unorganised Sector

Figure 1.2: Conventional brick production - problem tree

The central and state Governments are greatly concerned about top soil erosion towards the
production of massive quantities of bricks, in the background of enormous housing needs. The
ministry of power and the Government of India is thus promoting utilization of fly ash in the

3
production of construction materials by offering several incentives and making laws. But in
spite of that, due to mental barrier amongst the consumer and reluctance of the brick industry
to shift from conventional bricks to other material, techniques and process, entrepreneurial
activity has suffered. However, the ministry of environment & forest, Govt. Of India vide
notification no. S.O.763 (E) dated 14th September 1999 in term of para 3(2) and 3(3) and duly
supported by the urban development, Govt. of West Bengal vide letter no 2119(9)-
UD/N/M/D/M-1/95 dated 2nd June 2000 have prescribed the use of fly ash based brick in the
construction of building, drains, and bridges etc. Every Construction agency engaged in the
construction of building, bridges within the radius of 100 from coal and lignite based Thermal
Power Plants shall use fly ash brick or cement fly ash bricks (Ranjan 2012).
With the change of habits, choice as well as a change in society, the demand for a sustainable
alternative to conventional bricks is gradually increasing day by day not only in metro cities
but also in urban and rural areas. The unfired fly ash-sand-lime system of brick making has
gained popularity in India. Also, many potential uses of fly ash, which is a waste from thermal
power plants, in cement, paint, ceramic, and other applications to utilize and manage it are
identified and hence fly ash is a valuable waste material. One other waste generated from the
thermal power plant is pond ash, which is a mixture of bottom ash and fly ash. About 30% of
coal ash is handled wet and disposed as pond ash in nearby located ash bund. Possible
utilization of pond ash is reported in the literature as a partial replacement of fine aggregate in
concrete production, but is very limited due to pond ash is slightly finer in size than fine
aggregate and has higher water demand. Thus, this idea of using pond ash as the main system
in bricks can solve the issues related to its disposal which is presently causing ecological and
environmental problems.
To overcome the issues related to conventional bricks, utilization of various industrial waste
material in the brick making has gained much popularity in India and a many of these industrial
waste has been tried out successfully to produce bricks. But one major issue for their
commercial production is that there is no such standardised process or methodology available
for them like we have for the production of concrete, except for fly ash-sand-lime-gypsum
system which people have developed through experimentation over a long period of time based
on trial and error approach. This project aims to develop an unfired, non-structural, binder
bricks with 100% waste material using fly ash, pond ash, local industrial waste like coal cinder,
paper sludge, marble dust etc. along with lime and gypsum system to alleviate resources like
coal and diesel, preservation of topsoil, prevention of harmful emissions and simultaneously

4
managing the industrial waste (Figure 1.3 reflects the various benefits achieved through
proposed development of unfired bricks using industrial waste and their positive effects).

Improved Methodology in
Protection of Top-Soil Recycling Industrial By-Products

As a Green Building Effects

Low cost to End-User Component

Development of Unfired Brick Using Industrial Waste Objective

Low Energy Consumption in Environmental

Process (Unfired) Awareness through Recycling Causes

Saving of Natural Resources Utilization of Industrial Waste

Technological Advancement,
Organised Sector

Figure 1.3: Proposed brick production - objective tree

1.3 Research objectives

The research aims to fulfil following objectives:
1. To investigate maximum utilization of local industrial waste (fly ash, pond ash, coal cinder,
quarry dust, marble dust and paper sludge) for the development of non-structural, unfired,
binder bricks through extensive laboratory work.
2. To improve the compressive strength of bricks while optimizing binder content, weight
density, water absorption, and maximizing industrial waste utilization.
3. To identify variables affecting the various properties of brick.

5
1.4 Scope of work
To fulfil the aforementioned objectives of the research, following work packages are to be
covered:
 Characterize the raw materials to obtain their basic properties, composition and reactivity
for their possible utilization in bricks.
 Produce and analyse the commercially manufactured fly ash-stone dust-lime-gypsum
system as a base mix and its various engineering properties.
 Develop a basis for partial/complete replacement of stone dust with pond ash, fly ash with
pond ash and coal cinder, based on their packing density and its effect on various properties
of a brick compared to base mixes.
 Experiment and analyse the utilization of marble dust and paper sludge in order to achieve
optimum mix for brick production and compare it to the base mix.
 Identify the variables and develop a relationship for utilization of an industrial waste in
brick production.

1.5 Organisation of the thesis

The thesis has been divided into 6 chapters, tables & figures have been presented along with
the text wherever required. The overall outline of the thesis is summarized here;
 Chapter 1 gives a brief introduction with current scenario and the need for research.
 Chapter 2 deals with the literature review of the work done by various researchers in the
field of development of unfired bricks, optimization of process variables, and effect of
various industrial waste on brick properties.
 Chapter 3 explains about various constituent materials used in this study and their source
of generation and procurement.
 Chapter 4 provides detailed research methodology adopted to carry out this study, various
tests and experiments performed on the raw materials and casting methodology of
specimens.
 Chapter 5 deals with all the results obtained for various test performed and subsequent
discussion.
 Chapter 6 presents the summary of all the work done along with the major conclusions
drawn from this study. Future scope of the work is also discussed in this section.
 All the reference cited in this thesis are listed in the reference section.

6
 CHAPTER 2: LITERATURE REVIEW

2.1 General
Bricks are the main component of construction as far as residential building in concerned. It is
inevitable to use bricks in building construction. Due to large scale production and utilization
of bricks, it becomes evident that the brick industry presents an opportunity for the efficient
utilization of vast quantities of industrial waste which goes unmanaged and unutilized.
It’s beyond doubt that activity of primary industries often yields substantial amounts of by-
products. The disposal in the original industrial site is favoured by economic reasons, though
traditional storage in nearby dumps can be impractical owing to the considerable masses
involved and environmental restrictions. The local exploitation of these by-products is,
therefore, a growing technological aspect of basic industries and one tenable option is their re-
use as starting materials for other productions. For decades, bricks are mainly produced from
clay and shale, which causes substantial depletion of virgin resources due to the continuous
extraction of clay and removal of top soil for manufacturing of conventional bricks. Hence, in
recent years, civil engineers are obliged to find sustainable solutions for saving the virgin
resources by utilizing various industrial wastes.
So, as this huge amount of industrial by-product or wastes which are becoming a client for
increasing environmental pollution and generation of a huge amount of unutilized resources.
With a view to the above, this research is aimed at finding out utilization of such industrial by-
products for value-added applications in the development of bricks and also helps to solve the
environmental problems.

2.2 Production of conventional bricks

Bricks are one of the oldest known construction material, sometimes referred to as an artificial
stone. The earliest bricks are sun-dried bricks, dating back to 7000 BC in the Middle East and
South Asia. The production process and raw material involvement have not changed since the
first fired bricks production. The steps used then are used today, but with fine refinements. The
process of manufacturing involves; securing the clay, beneficiation, mixing and forming,
drying, firing and cooling. 99% of conventional clay bricks are produced through hand
moulding. After grounding, during soil-mix preparation water is added to soil; after water
addition, the typical moisture content of the mix is about 25 to 35% by weight. At this stage
fuels such as sawdust, powdered coal, etc. can be added to the mix, referred to as internal fuels.
The soil, water, and fuels are mixed into a homogenous mass. The mix is then moulded into

7
desired shape and size. The typical human energy requirement is estimated at 15 to 25 person
hours for moulding 1000 bricks.
The freshly moulded green bricks containing about 25% moisture by weight, are left in the
open, initially spread on the ground and later stacked in layers for natural drying to 3 to 15%
moisture. After that brick are subjected to fire. During firing, removal of mechanical moisture
takes place up to firing temperature less than 200°C, combustion of inherent carbonaceous
matter from 350°C to 700°C, endothermic decomposition of the clay molecules and
evaporation of chemically combined water from 400°C to 600°C.
Al2 O3 . 2SiO2 . 2H2 O = Al2 O3 + 2SiO2 + 2H2 O...………………………………………... (2.1)
Decomposition of calcium carbonate, a common impurity in soil, occurs at temperatures
ranging from 600°C to 800°C.
CaCO3  CaO + CO2 ……………………………………………………………………... (2.2)
The development of strength from mere soil particles to a strong and tough material is no
magic, it is basic chemistry. The action of heat gives rise to a sintering (vitrification) process
that causes the clay particles to fuse and thus develop extremely strong ceramic bonds in the
burnt clay bricks. Such bonds are highly stable, making the bricks highly resistant to severe
weathering actions and inert to normal chemical attacks. During vitrification new mineral
phases are formed, including liquid phases, which on cooling sets as glass phases and provide
strength to the fired brick. The typical chemical composition of brick is silica (50-60%),
alumina (20-30%), lime (2-5%), iron oxide (≤ 7%), magnesia (≤ 1%).

Forming Sintering

Raw powder Formed product Sintered product

Figure 2.1: Strength development mechanism (Sintering) of conventional fired clay bricks

Clay brick offers us all the advantages as artificial stone for decades, but with enormously
growing demand for construction it is not a viable solution to continue using conventional clay
bricks as very fertile land is deliberately eroded to meet the demand of clay brick for
construction. This devastating act is slowly killing our environment and we will be left with no
fertile land for agriculture in near future if it continues at the present rate. It is now high time
for us to collectively take the responsibility to take steps in the direction to develop and promote
utilization of sustainable alternatives to conventional clay bricks.

8
2.3 Fly ash bricks
Utilization of fly ash as a resource has been studied for decades in many areas such as in
environmental engineering, in ceramic products, in agriculture, in the paint industry, in
building products (brick, cement, aggregate). Fatih and Ümit (2001) carried out in-depth
experimentation to accommodate fly ash to replace clay from building bricks which were
usually made of a mixture of clay and sand by moulding, drying and burning in a kiln. They
conveyed that addition of fly ash up to 60%, at a firing temperature of 950°C is possible without
affecting the quality of brick at an optimum water content of 30% and compressive strength of
the range of 100 kg/cm2. The compressive strength of fly ash bricks is found to be increased
with increasing the temperature and decreasing the amount of fly ash as an additive, which may
be because of the insufficient plasticity of brick clay containing a high amount of fly ash.
A major breakthrough was achieved when Kayali (2005) conceived the idea of producing high
performance fired bricks with 100% fly ash as a solid ingredient opting for complete
replacement of conventionally used clay. He believed that fly ash on its own can be an excellent
raw material for brick making. Using similar equipment and technique as used for clay bricks,
the produced load bearing FlashBricks reported tremendous improvements in properties like
24% improvement in compressive strength, three times improved tensile strength, 44%
improvement in bond strength due to rougher texture, 28% reduction in density over good
quality clay bricks. Also, those bricks proved to be more durable, resistant to salt attack and
testified excellent resistance to sulphate attack. Thus paving the way for complete replacement
of conventionally used natural clay to support the preservation of agricultural top soil and way
to effectively manage more percentage of waste like fly ash.
With the growing demand for bricks by the construction industry and exhaustion of coal
reserves, which is required as a fuel for conventional production of bricks through the firing of
bricks into the kiln at high temperature. This firing process is not only energy intensive but also
adversely affect the landscape and causes high environmental pollution. For conventional burnt
bricks, it is estimated that the total energy usage (input) 4189.8 MJ/t with an output emission
of 202 kg CO2/t of brick. While the total energy usage for unfired bricks is around 657.1 MJ/t
with CO2 emission of 40.9 kg/t. An acute shortage of some novel approach was felt for
production of brick, which does not involve the high-temperature firing of bricks.
In 2013, Rai et al. prepared and characterised the lime activated unfired bricks named as FaL-
G using fly ash. The study showed that for a mix of fly ash (70%), sand (15%), lime (10%),
and gypsum (05%), crushing strength of 2.02, 3.17 and 5.32 MPa was obtained at 7, 14, and
21 days curing respectively with hand moulding. The SEM-EDXA results showed the initial
9
formation of CASH phase with free silica but as the curing time was increased other phases
like CSH, CAH etc. by reducing the free silica were responsible for further strength
development in bricks. The other main factor affecting the strength development was the
availability of water for reaction with an optimum moisture content of 25%. They also pointed
out that for curing unfired bricks only water ponding method gave sufficient strength as
compared other complicated curing method and which could be beneficial for lower capital
investment. For fly ash brick, it is well known that chemically pozzolanic reaction of fly ash
and lime occurs readily under thermal treatment creating strong structures with an increase of
mechanical strength. This reaction involves the formation of calcium silicate hydrate (CSH)
and calcium alumina-silicate hydrate (CASH) and enhances the strength of the bricks. The
formation of CASH in the initial stage is responsible for the initial strength gain and after
increasing curing time more new phases such as CSH were formed by utilizing free silica and
further increasing the strength. Also, the crushing strength could further be improved by
increasing moulding pressure.

2.4 Optimization of process parameters

Chaulia and Das (2008) carried out experimental probe to optimize the process parameters for
fly ash brick manufacturing like water to binder ratio, fly ash, coarse sand and stone dust by
Taguchi method with an objective function to maximize the compressive strength of brick as
compressive strength is a vital parameter to judge the stability and durability of the brick.
Taguchi parameter design method is a powerful tool for optimizing the performance
characteristic of a product. They used an L9 (34) orthogonal array to investigate 4 factors each
at 3 level with fly ash, coarse sand, stone dust and cement as raw material. The conclusions
illustrate that out of four process parameters water to binder ratio and stone dust had significant
effect on the compressive strength with optimum level of process parameter found to be water
to binder ratio of 0.4, fly ash of 39%, coarse sand of 24% and stone dust of 30% giving an
optimized compressive strength of 166.22 kg.cm-2 with a tolerance of ±10.97 kg.cm-2. Also,
their confirmatory experiment carried for the optimal condition has a compressive strength of
160.17 kg.cm-2. Figure 2.2 explains the effects of various process parameters on the
compressive strength of brick.

2.5 Effect of utilization of various industrial waste in bricks

Experimental and analytical work on possible utilization of various industrial by-
products/waste is widely reported.

10
In 2003, Weng et al. explored the possible utilization of dewatered and oven dried sludge as
brick materials. Results show the satisfactory addition of as much as 20% sludge at 960°C to
1000°C, although the optimum addition of 10% sludge with 24% moisture content in a moulded
mix and firing temperature of 880°C to 960°C.

Figure 2.2: Cause-and-effect diagram for processing of fly ash brick

In 2012, Rajput et al. produced the Waste Crete bricks by reuse of cotton (1-5%) and recycled
paper mill (89-85%) waste with cement (10%). The bricks manufactured were a bit lightweight
(half of that of conventional clay brick) due to the presence of tiny air pockets inside attributed
to paper waste. They also designed and fabricated a homogenizer and hand-operated hydraulic
press. They proposed the double stage press operation to preserve the surface smoothness on
drying. The strength development mechanism was a usual pozzolanic reaction. Although high
water absorption was also reported due to cellulosic nature of cotton waste.
In 2012, Bilgin et al. experimented and analysed the possible utilization of waste marble
powder in brick industry. They found that addition of marble dust addition has positive effects
on physical, chemical, and mechanical strengths of the produced industrial bricks. Marble dust
replacement varying from 0 to 80% have been tried out and 41×08×08mm rectangular prisms
specimens were cast at a forming pressure of 15 MPa. The results of this study depict that 10%
by weight of marble powder can be added with no sacrifice of technical properties. However,
more than 10% marble powder increases porosity, water absorption and decreases mechanical
properties.
Various researches have been carried out for effective utilization of pond ash in bricks. Vidhya
et al. (2013) carried out experimental studies on utilization of pond ash and fly ash bricks using
lime as an activator, sand to reduce laminar cracks in bricks, and gypsum to accelerate the
hardening process to obtain early strength. The important conclusions showed the average
compressive strength of 9.2 to 7.6 N/mm2 and increases with increase in lime content, average
water absorption of 10%, the weight density, water absorption values reduced with increasing

11
pond ash content, and no efflorescence was observed. The cost reduction of 20% was achieved
over conventional clay bricks.
Use of billet scale a by-product of the steel industry, an iron oxide formed on the surface of
steel during continuous casting is removed using water spray, was proposed by Shakir et al.
(2013), in brick production with fly ash, quarry dust and OPC as a binder. They proposed a
non-conventional method of brick production using a novel flowable method without pressing
and firing. The role of billet scale was more of a fine aggregate. The maximum compressive
strength reported was in the range of 23.3 to 16.0 MPa for cement content of 15% to 10%. The
higher strength was attributed to the fact that fly ash and quarry dust acted as a pozzolanic
material with SiO2 and Al2O3 reacting with Ca(OH)2 from hydration of cement to form CSH
and CASH making them chemically stable and structurally dense. Fly ash also reduces the
number of micropores. The results for UPV, water absorption, modulus of rupture, salt attack
and chloride attack were promising.
In 2013, Banu et al. experimented the fly ash-sand-lime system with gypsum addition to
produce unfired light weight structural bricks by obtaining an optimum mixture design as 55%
fly ash, 30% sand, and 15% hydrated lime with 14% gypsum. Efforts were also made to
optimize other process variables like forming pressure and curing condition. The optimum
forming pressure was to be 3000 psi. The significance of curing condition was also
demonstrated, as for optimum composition and pressure bricks cured for four weeks under
water followed by one week in air resulted in maximum strength of 877.36 kg/cm2 as compared
to the maximum compressive strength of 442.96 kg/cm2 when cured under spray water twice a
day for 5 weeks.
In 2014, Sumathi and Mohan carried out an experimental investigation to obtain the optimum
mix percentage of binder bricks using fly ash with the addition of lime, gypsum and quarry
dust using least quantity of binding material to achieve maximum compressive strength. They
obtained the optimum value of process parameters like water to binder ratio of 0.4, fly ash of
39%, coarse sand of 24% and stone dust of 30%. They portrayed the fact that lime reacts with
fly ash at normal temperature and forms calcium silicate hydrate having cementitious property
and is responsible for strength development in bricks. The optimum mix percentage of fly ash-
15%, lime-30%, gypsum-02% and quarry dust-53% provided a compressive strength of 7.91
N/mm2 and satisfied all other properties of fly ash bricks.
In 2015, Hwang and Huynh successfully demonstrated production of unfired building bricks
(UBB) using of unground rice husk ash (URHA) as a partial aggregate replacement (10-20%)
along with fly ash and cement (10-15%) as a binder with the application of densified mixture
12
design algorithm (DMDA). Forming pressure applied was 35 MPa. They managed to achieve
a fair compressive strength of 16.0 to 22.1 MPa, the flexural strength of 2.8 to 3.5 MPa, and
water absorption of 9.5 to 14.8% corresponding to 10 to 20% of URHA.
Naganathan et al. (2015) investigated the performance of bricks made by using fly ash and
bottom ash. Bricks were cast using a self-compacting mixture of fly ash, bottom ash, and
cement eliminating both firing and pressing. The compressive strength ranged from 7 to 17
MPa and strength increased with increase in fly ash. The peak value of strength was attained
for the mix with bottom ash to fly ash ratio of 1:1.25 and with bottom ash to cement ratio of
0.45. The optimum mix for BA:FA:C was found to be 1:1.25:0.45. UPV values ranged from
2.20 to 2.96 km/s, water absorption ranged from 12.6% to 29.2%, initial rate of suction (IRS)
ranged from 0.83 to 1.82 kg/mm2. All bricks developed in this investigation showed increased
fire resistance to the tune of 30% and durability in terms of corrosion resistance and increase
of weight were better compared to conventional clay bricks.

13
 CHAPTER 3: MATERIALS

3.1 General
In India total of 960 million tonnes of solid waste is generated every year. Out of which 350
million tonnes is organic in nature, 290 million tonnes inorganic waste and around 4.5 million
tonnes as hazardous in nature. These wastes are mainly the by-products of mining, agricultural,
municipal, industrial and other processes. In order to protect the environment; efforts should
be made to use the by-products waste generated from various sectors into some value-added
applications (Pappu et al. 2007). This chapter deals with the information, general characteristics
of the materials which are used in this research work. Fly ash, pond ash, coal cinder, paper
sludge, marble dust, lime, and gypsum are the material used.

3.2 Fly ash

Currently, India produces an enormous amount of fly ash of the order of more than 112 MT
(Pappu et al. 2007). According to a recent study by the Centre for Science and Environment
(CSE), fly ash disposal remains a major problem with only about 50 to 60% of the total fly ash
generated by the power sector being utilised in cement, concrete, bricks, in backfill or road
embankments, adhesives, wall boards, agriculture, paints etc. The remaining is dumped into
poorly designed and maintained ash ponds. As per estimates, about a billion tonne of these
toxic ash lies dumped in these ponds, polluting land, air, and water. By the year 2017, the
thermal power sector is estimated to produce 300 to 400 MT of fly ash a year and with that,
utilisation of all the fly ash being generated is going to become even tougher (Rai et al. 2013).
Fly ash is a by-product of the coal combustion in thermal power generation and consists mainly
of SiO2, Al2O3, Fe2O3, CaO, and some impurities. According to ASTM Standards, fly ash
belongs to class F if (SiO2+Al2O3+Fe2O3) > 70%, and belongs to class C if 70% >
(SiO2+Al2O3+ Fe2O3) > 50%. Usually, class F fly ashes have a low content of CaO and exhibit
pozzolanic properties, but class C fly ashes contain up to 20% CaO and exhibit cementitious
properties. A major part of fly ash is currently being utilized in cement and concrete production.
In concrete, it helps in improvement of mechanical strength and durability, the mechanism is
that when pozzolanic materials are added, calcium hydroxide Ca(OH)2 is transformed into
secondary calcium silicate hydrate (C-S-H) gel, causing the transformation of larger pores into
finer pores as a result of pozzolanic reaction of the mineral admixtures. Ca(OH)2, which
appears as a result of the hydration, affects the quality of the concrete negatively by forming
cavities because of its solubility in water and its low strength, although it helps in maintaining
the pH of the concrete. The use of mineral admixtures has a positive effect on the quality of

14
concrete by binding the Ca(OH)2 (Chaulia and Das 2008). A viable option for bulk utilization
of fly ash can be in production of bricks containing fly ash as a major ingredient. Because of
the low calcium content of fly ash used in this study, its behaviour is like a pozzolanic
admixture in the brick. In brick, it reacts with externally added lime to form the reaction
compounds.
Source: The fly ash was collected from Deepnagar Thermal Power Station, located near the
city of Bhusawal, Maharashtra with total production capacity of more than 1000 MW.

3.3 Pond ash

Pond ash is also a major residue generated during the combustion of coal in thermal power
plants. One of the most important cautions of World Bank to India is that disposal of coal ash
would require one meter square of land per person. In India, most of the thermal power plants
use a wet system for disposal of ash. When pulverized coal is burnt in a dry, bottom boiler,
about 70 percent of the ash is entrained in the flue gas and is captured and recovered as fly ash.
The remaining 30 percent of the ash is dry bottom ash, a dark grey, granular, porous material
that is collected in a water-filled hopper at the bottom of the furnace. It is collected wet and
pumped to ash ponds located nearby through pipes. The lagoon bottom ash is usually combined
with fly ash. This blended fly ash and bottom ash together is referred to as Pond Ash
(Ranganath et al. 1994). Ranganath R.V. (1996) studied the characteristics of ponded fly ash
in terms of its physical properties, chemical composition, mineralogical composition, and
morphology. He concludes that the method of disposal and process of ponding results in an
increase of loss on ignition values, a decrease in alkali oxides, a decrease in soluble silica
content, absence of smaller particles and presence of larger number of irregular coarser
particles, which contribute to reduced reactivity of ponded ash in comparison with dry fly ash.
Approximately 30 percent of the coal ash is handled wet and disposed of as Pond Ash.
Depending upon the boiler design and efficiency, the ratio of fly ash to bottom ash varies
between 70:30 and 80:20. The pond ash has appreciable carbon content responsible for high
water demand. Pond as differs from fly ash depending upon its particle size and zone of the
collection. It is coarser in size, with angular particles and very porous surface texture (Ganesh
et al. 2012).
Source: Pond ash was collected from Ash Bund located in Vellare village near Deepnagar
Thermal Power Station, Bhusawal, in the state of Maharashtra.

15
3.4 Stone dust
Stone dust is a by-product of the stone (granite) crushing process produced during quarrying
activities, is one of the materials that has recently gained an attention to be utilized as
concreting aggregates in plenty of applications like cement mortar, building block, concrete,
and in controlled low strength material (Shakir et al. 2013). Because of limited supply, the cost
of river sand has skyrocketed and its consistent supply cannot be guaranteed. Under this
circumstances use of manufactured sand becomes inevitable. Crushed sand, also known as M-
sand, stone dust, quarry dust etc., it is a residue taken from the stone quarry. Stone dust can be
an economic alternative to river sand. It is purpose made fine aggregate produced by crushing
and screening and further processing. It is the finest of the types of crushed stone. Usually,
stone dust is used in large scale in highways as a surface finishing material (Sumathi et al.
2014). Because of its ability to form a strong, non-porous surface, stone dust is often used in
between the stones or bricks in patios and walkways. The source of stone controls the chemical
composition of dust. The particles of stone dust are irregular, angular, and have rough and
crystalline surface texture. The particle size is nearly same to fine sand. Stone dust particles
have interlocking characteristics (Singh et al. 2016).
Source: Stone Dust (Crushed Sand) is collected from Burhanpur Stone Quarry, Burhanpur
(M.P.).

3.5 Coal cinder

Many industries such as paper mills, use coal as a fuel for firing boilers to generate steam. After
the coal is so burnt in the boilers, it leaves a residue known as "coal ash, or coal cinder" also
known as Bhuki or Rakhad by locals. It’s basically the powder or pieces from burned or
unburned coal that is not reduced to ashes but is incapable of further reduction. Coal cinder is
an inorganic waste produced in the combustion black coal in the boiler house. This by-product
can be a valuable resource, becoming an alternative to natural fines used in bricks and concrete.
Its use not only provides financial savings, but also savings of natural resources as well as
environmental profits resulting from reduced number of landfills. Coal cinder is an aggregate
of poor quality and low strength. Similar to fly ash, coal cinder has high silica content and low
calcium content. Coal cinder is characterised by large inhomogeneity and possibility of harmful
components (Smarzewski and Hunek 2016). The composition of coal cinder varies, depending
on the coal type, source, and burning condition.
Source: Coal cinder was collected from the NEPA Paper Mill, Nepanagar-Burhanpur (M.P.).
NEPA mill recorded a surplus of 1534 MT of coal cinder.

16
3.6 Paper sludge
In the recycled paper production, the process involves a number of filtration steps to maintain
the cellulose fiber as much as possible. However, as the cellulose fibres are broken, recycling
to manufacture new paper is only possible for 3 to 8 cycles, after which sludge is obtained. The
fraction that passes the final filter is regarded by the paper producers as waste paper sludge or
ETP sludge and is hence stockpiled. On the average, 35% of the material entering pulp and
paper mills becomes residue in forms of rejects. This residue contains about 40% organic and
60% inorganic components like calcite and other clayey materials (Scott and Smith 1995). The
residues are generally either deposited or burnt. Disposal of this residue is an important
environmental and economic problem for the paper industry. Various possible uses like
pozzolanic addition in cement manufacturing, glass ceramics, and as an organic pore-forming
agent in bricks are also reported. The major composition of paper sludge is CaO in the range
of 20 to 30%. The sludge composition, constituted mainly of calcite and kaolinite with a high
degree of purity, permits its possible reuse as a pozzolanic material (Garcia et al. 2008).
Source: Paper Sludge was collected from the NEPA Paper Mill, Nepanagar-Burhanpur (M.P.).
NEPA mill reports a surplus of approx. 668 MT of paper sludge every year.

3.7 Marble dust

Out of the total waste generated 6.5 million tonnes of waste is produced from marble industry.
There are two types of by-products generated from marble processing. Marble slurry i.e. water
containing marble powder and the other is stones of irregular shape or smaller size goes into
the scrap. One ton of marble slurry is said to be produced when one ton of marble stone is
processed. This dust produced is generally dumped near the river bed or nearby vacant pit, lead
to contamination of land, ground, and surface water. This undeniably leads to increase in
environmental risks as it dries up. The marble dust causes a reduction in permeability and
porosity of top soil resulting into water logging. This fine particle of marble dust reduces the
fertility of the ground surface due to increasing in alkalinity (Pappu, et al., 2007). As per the
status report of MSME Development Institute, Jaipur (Raj.), on commercial utilization of
marble slurry (2007), currently efforts are being made for utilization of marble dust as a filling
material for road and embankment, in manufacturing of cement, ceramic tiles, and concrete
aggregate, etc. Marble dust is chemically dolomitic in nature and consists of very fine particles.
Considering the physio-chemical properties, it may be used as a fine aggregate in
manufacturing of brick by using cement or lime as binders.
Source: Marble dust is collected from Rajasthan through TARA.

17
3.8 Quicklime
The name lime is used for both calcium oxide (quicklime) and calcium hydroxide (slacked
lime). When limestone (calcium carbonate) is heated, at about 1000°C, it undergoes thermal
decomposition. It loses carbon dioxide and turns into quicklime. The reaction is carried out in
specially constructed kilns. Limestone is added at the top and quicklime is removed from the
bottom in a continuous process. Humans have been aware of the steps needed to create
quicklime for a very long time, and chemists believe that its generation may be one of the oldest
chemical reactions known to man. People have certainly been using the material all over the
world for thousands of years. Quicklime requires careful handling. As it sits, it can acquire
carbon dioxide from the air, reverting to its original form. It has excellent binding properties.
It has been an important binding material in the construction industry since ages. There is a
wide range of uses for this substance, ranging from mortar to flux. Lime is indispensable for
use with mortar and plaster, in the manufacture of soap, rubber, varnish, refractories and lime
bricks etc. Lime react with fly ash at ordinary temperature and form a compound possessing
cementitious properties. After reaction between lime and fly ash, calcium-silicate-hydrates (C-
S-H) are produced which are responsible for the high strength of the compound.
Source: Procured from Jodhpur, Rajasthan through a local vendor from New Delhi.

3.9 Gypsum
Gypsum is a sedimentary soft sulphate mineral composed of calcium sulphate dehydrate
(CaSO4·2H2O). It’s a non-hydraulic binder occurring naturally as soft crystalline rock or sand.
Gypsum is having some important properties like rapid hardening and drying with negligible
shrinkage, small bulk density, good fire resistance, good sound absorbing properties, superior
surface finish etc. It can strengthen material or increase viscosity. Gypsum is used for
manufacture of wallboard, cement, plaster of Paris, soil conditioning, a hardening retarder in
Portland cement, brick making. Development of micro cracks has been observed particularly
in fly ash bricks without gypsum. The compressive strength of brick is reported to increase
with an increase in gypsum content to an optimum level. Gypsum is used to accelerate the
hardening process and obtaining the early strength in brick.
Source: Procured from a local supplier in New Delhi.

18
 CHAPTER 4: EXPERIMENTS

4.1 Research methodology

The experiments were carried out in three phases. After identification and collection of raw
materials, in the first phase of experiments physical and chemical characterizations of raw
material (Figure 4.1) was carried out based on their specific gravity, loss on ignition, water
absorption, Blaine’s fineness, particle size analysis, and XRD (X-Ray Diffraction). Also, check
for their reactivity were done through isothermal calorimetry and lime reactivity test.

Raw materials
characterization

Specific Loss on Water Blaine Particle size Isothermal Lime

XRD
gravity ignition absorption fineness analysis calorimetry reactivity

Figure 4.1: Raw material characterization

After successful characterization of constituent materials, in the second phase, casting of

specimens was carried out based on various blends of materials. Reactivity of raw material and
packing density formed the basis for mixture proportioning of blends. Initially casting of
commercially manufactured fly ash-stone dust-lime-gypsum brick system was based on the
optimum mix arrived from various literature reviews and market research and tested their
engineering performance. After that, attempts were made to study and analyse the effect of
partial to full replacement of stone dust with pond ash, fly ash with pond ash & coal cinder, in
the aforementioned brick system to observe the effect of packing density, and particle size
distribution along with maximum utilization of waste. After incorporating the changes in the
base mix, another optimum mix for fly ash-pond ash-lime-gypsum was made the reference to
compare the performance. Efforts were also made to study and analyse the effect of the addition
of paper sludge and marble dust in fly ash-pond ash-lime-gypsum system with an aim to
improve the compressive strength of brick while minimizing water absorption and weight
density. All the specimens were cured by water spraying & maintained at a temperature of
27°C. In the third phase, testing of all the specimens was carried out (Figure 4.2).

Tests on specimens

Mechanical strength Water absorption Density Efflorescence UPV

Figure 4.2: Tests on brick specimens

19
The specimens were tested for their compressive strength, ultrasonic pulse velocity, and water
absorption, to analyse the effects of replacement and addition of various waste with an aim to
identify the process variables affecting the various engineering properties of unfired bricks
developed by utilizing industrial waste. The size of test specimens was 5×5×5 cm with a fixed
percentage of lime, gypsum and mixing water to 9%, 3%, and 14% respectively. All the
specimens were tested for curing age of 3, 7, 14, 28 and 54 days.

4.2 Raw material characterization

Following sets of experiments were performed for characterization of constituent materials:
4.2.1 Specific gravity test
Specific gravity is normally defined as the ratio between the weight of a given volume of
material and weight of an equal volume of water. The specific gravity is the characteristic
generally used for calculation of the volume. It is important to determine the specific gravity
of raw materials, as it is the basic engineering property of a material, and also required to carry
out some other experiments like lime reactivity, Blaine’s fineness etc.
The specific gravity was determined as per the guidelines given in the IS 1727-1967, methods
of test for pozzolanic materials were employed for the determination of specific gravity of fly
ash, pond ash, coal cinder, paper sludge, marble dust, lime, and gypsum. Test procedures as
per IS 1122-1974 were followed for determination of specific gravity of crushed sand. For fly
ash, pond ash, coal cinder, paper sludge, and marble dust, specific gravity was measured by
‘Le chatelier’ Flask and for crushed sand pycnometer bottles were used (Figure 4.3).

Figure 4.3: 'Le chatelier' flask & Pycnometer bottle

Specific Gravity (G) for fly ash, pond ash, coal cinder, and paper sludge is calculated as the
ratio of the weight of sample poured into the ‘Le chatelier’ flask or pycnometer bottle to the
volume displaced by the sample. Table 4.1 lists the specific gravity of various raw materials
used.

20
 Table 4.1: Specific gravity of raw materials
Raw materials Specific gravity
Fly ash 2.18
Pond ash 2.03
Coal cinder 1.53
Paper sludge 1.23
Stone dust 2.85
Marble dust 2.88
Quicklime 2.29
Gypsum 2.46
4.2.2 Loss on ignition
Sequential loss on ignition (LOI) is a simple method for estimating the content of organic
matter and carbonate minerals in sediments using the linear relations between LOI values and
organic and inorganic carbon content. It consists of strongly heating ("igniting") a sample of
the material at a specified temperature, allowing volatile substances to escape, until its mass
ceases to change. Easy implementation in the laboratory makes the method widely used. The
method is based on differential thermal analysis: organic matter begins to ignite at about 200°C
and is completely depleted at about 550°C, and most carbonate minerals are destroyed at higher
temperatures (calcite between 800 and 850°C, dolomite between 700 and 750°C).

Figure 4.4: Muffle Furnace

This test was conducted as per the guidelines given in the IS 1727-1967. The samples of known
weight were taken into the ceramic crucibles and kept into the muffle furnace (Figure 4.4) first
at 100°C to remove the moisture, and then at 500°C, and 1000°C respectively for 2 hours of
exposure time, and change in weight was noted for each temperature. LOI was calculated as
the ratio of difference in initial weight of sample kept into the muffle furnace and the final

21
weight of sample after each stage to the initial weight of the sample, represented as a percentage
of initial weight. Table 4.2 shows LOI values for the raw materials used.
Table 4.2: Loss on ignition (LOI)
Loss on ignition (LOI)
Raw materials
100°C 500°C 1000°C
Fly ash 0.5% 1.3% 2%
Pond ash 0.2% 1.5% 1.6%
Coal cinder 0.8% 15.7% 17.0%
Paper sludge 4.0% 16.0% 58.0%
Stone dust 0.1% 0.4% 0.5%
Marble dust 0.0% 0.03% 2.34%
Quicklime 0.1% 0.21% 0.76%
Gypsum 0.1% 1.24% 1.79%
4.2.3 Water absorption test
It becomes inevitable to determine the amount of water absorption for new material like coal
cinder and paper sludge, as it is an important factor while performing other tests and production
of bricks. It is a simple but an important test to determine the water absorption of raw material
up to the saturation level.

Figure 4.5: Water absorption test

In this test, the collected materials were immersed into the water for 24 hours and then a sample
of known weight was kept into the laboratory oven at a temperature of 100±5°C for next 24
hours for drying. Table 4.3 denote the values of water absorption for all the waste used in the
production of the brick specimen.
Table 4.3: Water absorption of raw materials
Raw materials Water absorption (%)
Coal cinder 9.11%
Paper sludge 70.8%
Stone dust 0.97%

22
The change in weight with respect to original weight was represented as water absorbed by the
material and same water correction was also applied while using them in the preparation of
bricks and other tests. The water absorption of a material was given as the difference in
saturated weight of sample and oven dried weight of the sample, expressed as a percentage of
the saturated weight of the sample.
4.2.4 Blaine’s fineness test
The fineness is one of the primary physical characteristics other than the sieve analysis,
fineness is defined by the specific surface area determined by Blaine’s air permeability
apparatus (Figure 4.6). The apparatus consists essentially of a means of drawing a definite
quantity of air through a prepared bed of definite porosity. The number and size of the pores in
prepared bed of sample of definite porosity (e = 0.5±0.005) is a function of the size of the
particles and determines the rate of air flow through the bed.

Figure 4.6: Blaine’s air permeability test apparatus

The test was conducted as per the guidelines given in the IS 1727-1967. The bulk volume of
compacted bed of sample was determined by mercury displacement method. The obtained
weight of the sample was filled into the permeability cell with a perforated metal disk at the
base, which was covered with filter paper. The cell was covered by pressing the plunger softly
by the thumb and the assembly was kept on Blaine’s apparatus.
A digital display unit showed the results in terms of specific surface area of the sample material
correlated as a product of instrument constant (k = 83.5, for fly ash) and the square root of time
23
taken to pass the air through a bed of specific porosity. Table 4.4 provides the fineness of raw
material used. This test was not performed for paper sludge due to it its flaky behaviour.
Table 4.4: Fineness (Blaine’s value) for raw materials
Raw materials Specific surface area (Blaine’s value), (m2/kg)
Fly ash 334.4
Pond ash 182.1
Coal cinder 271.8
Marble dust 379.4
Quicklime 376.4
Gypsum 332.9

4.2.5 Image Analysis

Image analysis is the extraction of meaningful information from digital images with the help
of digital image processing techniques. Image analysis is a powerful tool when various
characteristics of the material such as particle shape, size, texture, morphology, etc. are
required to understand its behaviour.
The test could be divided into three steps: sample preparation, image acquisition, and image
processing. This test was performed for crushed sand, pond ash, coal cinder, and paper sludge.
For fly ash, marble dust, quicklime, and gypsum, this test was not carried out, due to very fine
particle size requiring very higher resolution.
Sample Preparation: The sample material was taken using quadrupling method, and washed
off in 75 micron IS sieve for removing very fine particles adhered to the surface due to
electrostatic forces. After that, the specimen was dried for 24 hrs in a laboratory oven.
Image Acquisition: This was done with the help of a high resolution scanner (HP Scanjet
G4010). The particles were scattered and spread on a transparent plastic sheet with a small gap
between the particles to avoid overlapping of particles. The particles were covered by a red
fluorescent sheet for the background. The resolution was set to 4800 dpi in order to take care
of smaller particles.
Image Processing: Scanning Probe Image Processor (SPIP version. 6.4.4) was proposed to be
used for the analysis of scanned image by choosing appropriate parameters and options. But
due to unavailability of software, this part was left incomplete. Although, the images acquired
(Figure 4.7) were useful for the understanding the particle size, shape, and texture of the
specimen.

24
 (a) (b)

(c) (d)

Figure 4.7: Image analysis {(a). Stone dust, (b). Pond ash, (c). Coal cinder, (d). Paper sludge}
4.2.6 X-ray powder diffraction (XRD)
X-ray powder diffraction (XRD) is a rapid analytical technique used to obtain information
about the structure of crystalline materials. XRD is primarily used for the identification and
characterization of compounds based on their diffraction pattern. By scanning the sample
through a range of 2θ angles, all possible diffraction directions of the lattice should be attained
due to the random orientation of the powdered material. Conversion of the diffraction peaks to
d-spacing allows identification of the mineral because each mineral has a set of unique d-
spacing. Typically, this is achieved by comparison of d-spacing with standard reference
patterns.
Working of X-ray diffractometer is based on constructive interference of monochromatic X-
rays and a crystalline sample. A cathode ray tube generates the X-ray, which is then directed
toward the sample. Incident rays interact with the sample to produce constructive interference
when conditions satisfy Bragg's Law (nλ=2d sin θ) and a diffracted ray results. Bragg’s law
relates the wavelength of electromagnetic radiation to the diffraction angle and the lattice

25
spacing in a crystalline sample. X-ray diffractometers generally consist of three basic elements:
An X-ray tube, a sample holder, and an X-ray detector. X-rays are generated in a cathode ray
tube by heating a filament to produce electrons, accelerating the electrons toward a target by
applying a voltage, and bombarding the target material with electrons. When electrons have
sufficient energy to dislodge inner shell electrons of the target material, characteristic X-ray
spectra are produced. Copper is the most common target material. These X-rays are collimated
and directed onto the sample. As the sample and detector are rotated, the intensity of the
reflected X-rays is recorded. When the geometry of the incident X-rays impinging the sample
satisfies the Bragg Equation, constructive interference occurs and a peak in intensity occurs. A
detector records and processes this X-ray signal and converts the signal to a count rate which
is then output to a device such as a printer or a computer monitor.
Bookers XRD, D8-ADVANCE was used for the experiments (Figure 4.9). A few gram of
sample material, as pure as possible, was obtained and grounded to fine powder. The grounded
samples were placed into the sample holder (Figure 4.8). The sample holders were placed into
the XRD machine, assuring a flat upper surface with the help of glass slide and X-ray
diffractometer was started. The results obtained were analysed with the help of X’Pert
Highscore Plus software.
Following are the XRD results obtained for fly ash, pond ash, coal cinder, paper sludge, marble
dust, quicklime, and gypsum (Figure 4.10 to Figure 4.17). They depict the various crystalline
phases present in the raw materials.

Figure 4.8: XRD sample preparation & placement

26
Figure 4.9: X-Ray Diffractometer (Bookers XRD, D8-ADVANCE)

Figure 4.10: XRD result for fly ash

Figure 4.11: XRD result for pond ash

27
Figure 4.12: XRD result for stone dust

Figure 4.13: XRD result for marble dust

Figure 4.14: XRD result for coal cinder

28
Figure 4.15: XRD result for Paper Sludge

Figure 4.16: XRD result for quicklime

Figure 4.17: XRD result for gypsum

29
4.3 Reactivity of raw materials
4.3.1 Lime Reactivity
Lime reactivity is a standard test for determining the reactivity of the pozzolanic material with
hydrated lime, as represented by compressive strength of standard mortar test cubes prepared
and tested under specific conditions.
The test was conducted in accordance with the guidelines given in the IS 1727-1967. The dry
materials of the standard test were lime: pozzolan (fly ash, pond ash, coal cinder, and paper
sludge): standard sand. They were mixed with water, in the proportion of 1:2M:9 by weight.
Where M was the ratio of the specific gravity of pozzolana and specific gravity of slacked lime.
The amount of water to be added was calculated from the flow table test as per IS 5512-1983.
Various water contents were tried. And the water content which on flow table gave the flow
dia of 17±5 cm with 10 drops in 6 seconds was taken as the water content for the mix.

Figure 4.18: Flow table test for lime reactivity

The prepared mix was poured into the standard cube moulds of 5 cm size. After initial air
curing of 48 hours, specimens were demoulded and cured at 50±2°C with a relative humidity
of 90 to 100%, for next 8 days. Table 4.5 shows the lime reactivity results for fly ash, pond
ash, coal cinder, and paper sludge.
Table 4.5: Lime reactivity of raw materials
Raw materials Lime reactivity (kg/cm2)
Fly ash 2.62
Pond ash 1.77
Coal cinder 2.92
Paper sludge 1.87

30
4.3.2 Isothermal calorimetry
The pozzolanic reaction is an exothermic process. Measuring the heat released during the
reaction indirectly refers to the kinetics of the reaction and it is an indirect way to find out the
reactivity of a material. In this test, the heat flow from the specimen is studied which is
maintained at a near isothermal condition by maintaining contact with a heat sink.
Isothermal Calorimeter (Calmetrix I-Cal8000) was used for the test. The temperature of the
mix components was regulated to the ambient temperature by keeping them in the working
environment at least 24 hours before use. Similarly in the case of the calorimeter for the
temperature to stabilize to the levels required. The mix components were weighed as per the
blend ratios planned (Table 4.6) by means of a high precision weighing machine. The activator
(Slacked lime) was added to the dry sample and mixed thoroughly until the resulting paste of
uniform consistency was obtained. The paste was then transferred into an oiled plastic
container which was to be placed in the isothermal calorimeter (isocal) channels.
Table 4.6: Blends for isothermal calorimetry
Mix ID Sample Water/Sample ratio Activator (Lime)
C1 Fly ash (FA)
C2 Pond ash (PA)
C3 Coal cinder (CC) 0.5 10%
C4 Paper sludge (PS)
C5 FA+PA (1:1)

180
Cummulative Energy (J/g)

160
140
120 Fly Ash
100 Pond Ash
80
Coal Cinder
60
40 Paper Sludge
20 FA+PA (1:1)
0
0:00 4:48 9:36 14:24 19:12 24:00
0:00
Time (hours)

Figure 4.19: Isothermal calorimetry results

The computer attached to the isocal was started immediately for logging of heat flow and
software connected to the isocal automatically recorded the readings from heat sensors and

31
stored the data for future reference. Energy values were also recorded, which were retrieved
after the required time period (3 days) was complete. Results were represented by plotting a
graph of cumulative energy released per gram of mix with respect to time, as represented above
in Figure 4.19.

4.4 Casting of specimens

4.4.1 Mixture proportioning of specimens
The mixture proportioning of different blends with varying proportions of the constituent
materials was carried out based on the characterization of raw materials, and through a
literature survey. The base mix (BM) for ‘fly ash-stone dust-lime-gypsum’ system was as per
the optimized mix developed by a for-profit organisation “Technology and Action for Rural
Advancement” (TARA) for commercial production of fly ash bricks and through a literature
survey. In the base mix, fly ash (50%) and stone dust (50%) were the major constituents, where
fly ash the reactive component and stone dust acted as strong inert filler and interlocking
material. Lime (9%), and gypsum (3%) were acting as a binder and catalyst, respectively. The
water percentage for mixing was fixed at 14% by weight of constituents, and correction for
water absorbing materials was applied, wherever required. To establish a common evaluation
basis, the variations in the blend were done in such a way that when one of the constituent
material was replaced then the original material’s proportion was increased or decreased in the
same proportion and all the other constituent’s proportions were kept same.
In the first set of variation, an attempt was made for complete replacement of the stone dust
with pond ash, in order to augment the utilization of underutilized by-product from coal-based
thermal power plants. The blends varied with an increase in the percentage of pond ash from
0% to 50% and simultaneously, decrease in the percentage of stone dust from 50% to 0%, with
a variation of 12.5% in each next blend. This variation resulted in the development of ‘fly ash
pond ash-lime-gypsum’ system of brick production. This blend will act as a reference mix
(RM) from here onwards.
Table 4.7: Blends for replacement of stone dust from base mix with pond ash
Fly Stone Quick
Series Mix ID Pond ash Gypsum Water
ash dust lime
PA-0% (BM) 50% 50% 0%
PA-12.5% 50% 37.5% 12.5%
A PA-25% 50% 25% 25% 9% 3% 14%
PA-37.5% 50% 12.5% 37.5%
PA-50% (RM) 50% 0% 50%

32
Further, in the second set of blends, an attempt was made to maximize the use pond ash. Fly
ash from this reference mix was also replaced with pond ash. This was achieved by a decrease
in the percentage of fly ash from 50% to 0% and simultaneously increase the percentage of
pond ash from 50% to 100%, with a variation of 12.5% in each set of next blend.
Table 4.8: Replacement of fly ash from reference mix with pond ash
Series Mix ID Fly ash Stone dust Pond ash Quick lime Gypsum Water
PA-50% (RM) 50% 0% 50%
PA-62.5% 37.5% 0% 62.5%
B PA-75% 25% 0% 75% 9% 3% 14%
PA-87.5% 12.5% 0% 87.5%
PA-100% 0% 0% 100%
As from aforementioned tests, based on the lime reactivity and isothermal calorimetry, coal
cinder showed promising reactivity amongst all the other waste materials. In the third set of
blends, an attempt was made to utilize the coal cinder by replacing the fly ash (reactive
component) from the reference mix with coal cinder by following the similar variation. This
resulted in the development of ‘coal cinder-pond ash-lime-gypsum’ system of brick production.
Table 4.9: Replacement of fly ash from reference mix with coal cinder
Series Mix ID Fly ash Pond ash Coal cinder Quick lime Gypsum Water
RM 50% 50% 0%
CC-12.5% 37.5% 50% 12.5%
C CC-25% 25% 50% 25% 9% 3% 14%
CC-37.5% 12.5% 50% 37.5%
CC-50% 0% 50% 50%
Now in the fourth set of blends, the addition of paper sludge was attempted with a view to
achieve internal curing of bricks due to its higher water absorption capacity. In the reference
mix, paper sludge was added with an increased amount of 10%. But after 30% addition of paper
sludge, it became practically impossible to prepare the specimens due to its flaky shape and the
specimens were getting disintegrated. Thus, only three blends with an increasing variation of
10% were prepared.
Table 4.10: Addition of paper sludge to the reference mix
Series Mix ID Fly ash Pond ash Paper Sludge Quick lime Gypsum Water
RM 50% 50% 0%
PS-10% 50% 50% 10%
D 9% 3% 14%
PS-20% 50% 50% 20%
PS-30% 50% 50% 30%

33
At last, addition of marble dust in the reference mix of ‘fly ash-pond ash-lime-gypsum’ system
was attempted. In order to utilize the marble dust to improve the packing density of the blends
due to a fine particle size of marble dust, and to achieve pore refinement. Due to a shortage of
time, only three blends with increasing additions of 10% were prepared. Shows the mixture
proportions of all the blends prepared for this study.
Table 4.11: Addition of marble dust to the reference mix
Series Mix ID Fly ash Pond ash Marble dust Quick lime Gypsum Water
RM 50% 50% 0%
MD-10% 50% 50% 10%
E 9% 3% 14%
MD-20% 50% 50% 20%
MD-30% 50% 50% 30%
4.4.2 Casting methodology
Cubical brick specimens of 5×5×5 cm were prepared with a forming pressure of 15 MPa. The
pressure of 15 MPa was applied with the help of digital compression testing machine (CTM)
with 3.73kN load at a rate of 0.9 kN/sec. The raw materials were freshly mixed in
predetermined mixture proportion in an automatic concrete mixer of 20-litre capacity. The
casting moulds were kept ready with oil lubrication. The fresh mix was firstly placed into the
cubical cast iron mould with hands and pressed with fingers and thumb. Then, the hand pressed,
filled mould was overfilled to create a hump of material over it. The overfilled mould was kept
in between the jaws of CTM and the pressure was applied to it. The uneven layer of material
in the CTM pressed mould was levelled with the help of a trowel.

Figure 4.20: Casting of various brick specimens

34
Figure 4.20 shows specimens cast for various blends. The specimens were demoulded after 3-
4 hours. The curing was done by wrapping the specimens inside the gunny bag, and sprinkling
with water to mimic the actual curing condition. A curing temperature of 27°C with a relative
humidity of 50 to 70% was maintained in the chamber. More than 900 successful brick
specimen from 20 blends, were prepared for the execution of various tests.

35
 CHAPTER 5: RESULTS & DISCUSSION

5.1 Results
5.1.1 Compressive strength test
Compressive strength is the most important test for assuring the engineering quality of bricks.
This test was performed in accordance with IS 3495(Part 1)-1992. All the prepared brick
specimen for blends of series A, B, C and D were tested for their compressive strength at the
curing age of 3, 7, 14, 28, and 54 days. For blends of series E, 54 days compressive strength
test was not performed due to a shortage of time. Minimum of three samples was tested at each
test age. This test was performed by using automatic Compression Testing Machine (CTM) of
capacity 5000kN by applying a constant progressing load at the rate of 0.6 kN/sec (Figure 5.1).
Compressive strength (MPa) was calculated as the ratio of ultimate failure load to the area of
sample perpendicular to the direction of application of load.

Figure 5.1: Compression testing machine

Compressive strength test results for series A, for blends replacing stone dust from the base
mix (BM) with pond ash, are shown in Table 5.1.
Table 5.1: Compressive strength (MPa) results at different ages for replacement of stone dust
from base mix with pond ash (Series A)
Series Mix ID 3 Days 7 Days 14 Days 28 Days 56 Days
PA-0% (BM) 0.282 1.239 5.137 9.311 16.516
PA-12.5% 0.312 1.051 4.160 7.183 15.521
A PA-25% 0.264 0.904 3.207 6.723 13.017
PA-37.5% 0.278 1.040 2.139 6.155 10.920
PA-50% (RM) 0.293 1.045 2.813 5.278 8.282

36
 Table 5.2: Compressive strength (MPa) results at different ages for replacement of fly ash
from reference mix with pond ash (Series B)
Series Mix ID 3 Days 7 Days 14 Days 28 Days 56 Days
PA-50% (RM) 0.293 1.045 2.813 5.278 8.282
PA-62.5% 0.384 0.975 3.218 4.263 6.390
B PA-75% 0.363 0.987 2.515 3.185 5.845
PA-87.5% 0.371 0.934 2.314 2.975 4.665
PA-100% 0.379 0.512 1.614 2.128 3.079
Table 5.3: Compressive strength (MPa) results at different ages for replacement of fly ash
from reference mix with coal cinder (Series C)
Series Mix ID 3 Days 7 Days 14 Days 28 Days 56 Days
PA-50% (RM) 0.293 1.045 2.813 5.278 8.282
CC-12.5% 0.635 1.511 3.362 4.125 7.179
C CC-25% 0.502 0.792 2.738 3.906 5.209
CC-37.5% 0.489 1.019 1.898 3.287 5.313
CC-50% 0.629 1.195 2.562 3.794 4.617
Table 5.4: Compressive strength (MPa) results at different ages with addition of paper sludge
to the reference mix (Series D)
Series Mix ID 3 Days 7 Days 14 Days 28 Days 56 Days
PA-50% (RM) 0.293 1.045 2.813 5.278 8.282
PS-10% 0.691 1.650 2.358 3.397 3.701
D
PS-20% 0.385 0.461 0.695 0.848 1.476
PS-30% 0.308 0.345 0.485 0.508 0.914
Table 5.5: Compressive strength (MPa) results at different ages with addition of marble dust
to the reference mix (Series E)
Series Mix ID 3 Days 7 Days 14 Days 28 Days 56 Days
PA-50% (RM) 0.293 1.045 2.813 5.278 8.282
MD-10% 1.062 3.665 9.835 13.014 NA
E
MD-20% 0.837 2.418 6.707 9.722 NA
MD-30% 1.137 2.747 8.065 11.664 NA
5.1.2 Ultrasonic pulse velocity test (UPV)
The pulse velocity in a material depends on its density and its elastic properties which affect
the quality and the compressive strength of material. UPV is aimed at estimating the likely
compressive strength, uniformity, homogeneity, and quality of bricks; detection of the presence
of cracks, voids, and other imperfections & measurement of elastic modulus and various other
properties.

37
IS 13311(Part-1):1992 governs the UPV test on concrete and the same procedure was followed
here. Although, the results were compared with existing results for bricks available from the
literature. UPV apparatus (Figure 5.2) was first calibrated using a reference carbon rod and
then a layer of grease was applied on the two opposite smooth faces of the specimen and on
the surface of transducers to have an air tight connection. Transducer was then placed on the
opposite faces of the specimen and reading from the display unit represented the transit time.
Minimum of three samples was tested at each test age. The ultrasonic pulse velocity (V,
km/sec) is calculated as the ratio of travel length (length of the specimen) to the transit time.

Figure 5.2: UPV apparatus

Table 5.6 shows results of ultrasonic pulse velocity (km/s) (UPV), for blends containing a
replacement of stone dust from the base mix with pond ash. UPV results for series B and series
C blends having a replacement of fly ash from the reference mix with pond ash and coal cinder
are represented in Table 5.7 and Table 5.8, respectively. Table 5.9 and Table 5.10 are showing
the UPV results for addition of paper sludge and marble dust to the reference mix, respectively.
Table 5.6: UPV (km/s) results at different ages for replacement of stone dust from base mix
with pond ash (Series A)
Series Mix ID 3 Days 7 Days 14 Days 28 Days 56 Days
PA-0% (BM) 1.73 1.97 2.29 2.52 2.82
PA-12.5% 1.55 1.82 1.91 2.27 2.73
A PA-25% 1.29 1.61 1.85 2.17 2.40
PA-37.5% 1.45 1.56 1.88 2.06 2.29
PA-50% (RM) 1.46 1.68 1.97 2.13 2.20
Table 5.7: UPV (km/s) results at different ages for replacement of fly ash from reference mix
with pond ash (Series B)
Series Mix ID 3 Days 7 Days 14 Days 28 Days 56 Days
PA-50% (RM) 1.46 1.68 1.97 2.13 2.20
PA-62.5% 1.52 1.73 2.00 2.15 2.25
B PA-75% 1.36 1.74 1.85 2.06 2.21
PA-87.5% 1.31 1.74 1.63 1.88 2.19
PA-100% 1.16 1.30 1.51 1.64 1.86

38
Table 5.8: UPV (km/s) results at different ages for replacement of fly ash from reference mix
with coal cinder (Series C)
Series Mix ID 3 Days 7 Days 14 Days 28 Days 56 Days
PA-50% (RM) 1.46 1.68 1.97 2.13 2.20
CC-12.5% 1.15 1.17 1.53 1.66 1.91
C CC-25% 1.07 1.26 1.25 1.50 1.56
CC-37.5% 0.94 0.93 1.05 1.30 1.38
CC-50% 0.96 0.93 1.07 1.25 1.32
Table 5.9: UPV (km/s) results at different ages for addition of paper sludge to the reference
mix (Series D)
Series Mix ID 3 Days 7 Days 14 Days 28 Days 56 Days
PA-50% (RM) 1.46 1.68 1.97 2.13 2.20
PS-10% 0.80 0.86 0.83 0.85 0.90
D
PS-20% 0.65 0.67 0.68 0.69 0.71
PS-30% 0.54 0.56 0.57 0.56 0.58
Table 5.10: UPV (km/s) results at different ages for addition of marble dust to the reference
mix (Series E)
Series Mix ID 3 Days 7 Days 14 Days 28 Days 56 Days
PA-50% (RM) 1.46 1.68 1.97 2.13 2.20
MD-10% 1.47 2.11 2.62 2.75 NA
E
MD-20% 1.11 1.97 2.32 2.47 NA
MD-30% 1.52 2.07 2.58 2.59 NA
5.1.3 Water absorption & bulk density test
Water absorption is the main factor affecting the durability of bricks. Less the water infiltrates
into the brick, the more durable the brick, and a higher resistance to natural environment is
expected. Thus, the internal structure of brick should be dense enough to avoid the intrusion of
water. The bulk density of brick is defined as the ratio of the weight of brick to the volume of
the brick.
Water absorption test was performed as per the guidelines given in IS 3495 (Part 2):1992, also
known as 24-hr immersion cold water test. This test was performed by placing the specimen
into the laboratory oven at a temperature of 100 ± 5°C for 24 hours till it attains substantially
constant mass. The specimen from the oven were immersed into the water for 24 hours at a
temperature of 27 ± 2°C. Change in weight with respect to original weight was represented as
water absorbed by the specimen. Minimum of three samples was tested at each test age and the
average value represented the water absorption percentage. The bulk density was calculated by

39
dividing the dry weight of specimen with direct volume measurement (length-height-width) of
unfired specimens. Minimum of three samples was tested at each test age and the average
values were represented as the bulk density of the specimen.
Table 5.11 to Table 5.15, shows the result of average water absorption and bulk density for
various blends from series A to series E, respectively.
Table 5.11: Average water absorption (%) and bulk density results for replacement of stone
dust from base mix with pond ash (Series A)
Series Mix ID Water absorption (%) Bulk density (g/cc)
PA-0% (BM) 15.4% 1.69
PA-12.5% 16.1% 1.56
A PA-25% 18.2% 1.49
PA-37.5% 19.1% 1.43
PA-50% (RM) 19.8% 1.34
Table 5.12: Average water absorption (%) and bulk density results for replacement of fly ash
from reference mix with pond ash (Series B)
Series Mix ID Water absorption (%) Bulk density (g/cc)
PA-50% (RM) 19.8% 1.34
PA-62.5% 20.6% 1.32
B PA-75% 22.0% 1.28
PA-87.5% 23.6% 1.23
PA-100% 26.9% 1.12
Table 5.13: Average water absorption (%) and bulk density results for replacement of fly ash
from reference mix with coal cinder (Series C)
Series Mix ID Water absorption (%) Bulk density (g/cc)
PA-50% (RM) 19.8% 1.34
CC-12.5% 20.4% 1.31
C CC-25% 20.6% 1.25
CC-37.5% 23.3% 1.16
CC-50% 23.8% 1.10
Table 5.14: Average water absorption (%) and bulk density results for addition of paper
sludge to the reference mix (Series D)
Series Mix ID Water absorption (%) Bulk density (g/cc)
PA-50% (RM) 19.8% 1.34
PS-10% 25.5% 1.17
D
PS-20% 28.6% 1.04
PS-30% 35.0% 0.85

40
Table 5.15: Average water absorption (%) and bulk density results for addition of marble dust
to the reference mix (Series E)
Series Mix ID Water absorption (%) Bulk density (g/cc)
PA-50% (RM) 19.8% 1.34
MD-10% 15.4% 1.53
D
MD-20% 17.7% 1.51
MD-30% 14.1% 1.57
5.1.4 Efflorescence test
Efflorescence is a fine, white, powdery deposit of water-soluble salts left on the surface of
bricks as the water evaporates. This test was conducted as per the guidelines given in IS 3495
(Part 3):1992. For this test, specimen were placed in water with one end immersed. The depth
of immersion for water being 2.5 cm. This arrangement was then placed in a warm (20-30°C)
and well-ventilated room until all the water is absorbed by the specimen and the surplus water
evaporates. Care was taken to prevent excess evaporation by covering the arrangement with
glass. After complete evaporation of water, the same procedure was repeated ones again.
Results were reported after second evaporation. As per the IS code, based on the percentage of
exposed area covered with thin deposit of salt, as inspected visually, the liability of
efflorescence was reported as nil (0%), slight (not more than 10%), moderate (up to 50%),
heavy (more than 50%), and serious (powdering & flaking of surface). This test was performed
at the age of 28 days.

5.1.5 Initial porosity

Initial porosity (P) for the brick specimens was determined in order to observe the effect of
voids present in the specimen. Initial porosity was determined as the ratio of pore volume (VP)
to the total volume (VT) of the specimen. Initial pore volume was calculated as the difference
between the total volume and solid volume (VS) of the ingredients of the specimen.
𝑉𝑇 −𝑉𝑆
𝑃= × 100 (%)…………………………………………………………………….. (5.1)
𝑉𝑇

Table 5.16 shows results of initial porosity (%) for blends containing a replacement of stone
dust from the base mix with pond ash. Initial porosity results for series B and series C blends
having replacement of fly ash from the reference mix with pond ash and coal cinder are
represented in Table 5.17 and Table 5.18, respectively. Table 5.19 and Table 5.20 are showing
the porosity results for the addition of paper sludge and marble dust to the reference mix,
respectively.

41
Table 5.16: Initial porosity results for replacement of stone dust from base mix with pond ash
(Series A)
Series Mix ID Initial porosity (%)
PA-0% (BM) 3.29%
PA-12.5% 8.89%
A PA-25% 8.17%
PA-37.5% 7.26%
PA-50% (RM) 14.26%
Table 5.17: Initial porosity results for replacement of fly ash from reference mix with pond
ash (Series B)
Series Mix ID Initial porosity (%)
PA-50% (RM) 14.26%
PA-62.5% 25.77%
B PA-75% 25.61%
PA-87.5% 24.69%
PA-100% 35.07%
Table 5.18: Initial porosity results for replacement of fly ash from reference mix with coal
cinder (Series C)
Series Mix ID Initial porosity (%)
PA-50% (RM) 14.26%
CC-12.5% 16.92%
C CC-25% 16.79%
CC-37.5% 22.48%
CC-50% 29.26%
Table 5.19: Initial porosity results for addition of paper sludge to the reference mix (Series D)
Series Mix ID Initial porosity (%)
PA-50% (RM) 14.26%
PS-10% 29.97%
D
PS-20% 28.19%
PS-30% 35.92%
Table 5.20: Initial porosity results for addition of marble dust to the reference mix (Series E)
Series Mix ID Initial porosity (%)
PA-50% (RM) 14.26%
MD-10% 5.91%
D
MD-20% 3.94%
MD-30% 1.52%

42
5.2 Discussion
5.2.1 Compressive strength test
Compressive strength decreases with increasing percentage replacement of stone dust with
pond ash in series A for all ages. With an aim to utilize pond ash instead of stone dust, the
complete replacement of stone dust from the base mix (fly ash-stone dust-lime-gypsum) results
in 50% reduction of compressive strength at the age of 56 days as shown in Figure 5.3. It can
be explained as pond ash in porous in nature and finer than the stone dust. Also, stone dust is
strong in nature, which acts as aggregates in the brick system, and may create voids in the
system when replaced solely. It can also be explained as the initial porosity of the system
increased from 3.29% to 14.26%.
It is noted that there is a substantial increase in the compressive strength from 28 days to 56
days. This can be explained by the observations made by Rai et al. (2013) that after initial
formation of CASH phase which is responsible for initial strength gain, with further increase
in curing time, formation of other phases like CSH, CAH etc. are responsible for further
strength development in bricks by reduction of free silica.
18
Compressive strength (MPa)

16
14
12 3 Days
10
7 Days
8
14 Days
6
4 28 Days
2 56 Days
0
Base Mix PA-12.5% PA-25% PA-37.5% PA-50%
(BM)
Series A

Figure 5.3: Compressive strength (MPa) for replacement of stone dust with pond ash in base
mix
Similarly, for the replacement of fly ash from the reference mix (fly ash-pond ash-lime-
gypsum) with pond ash and coal cinder, the compressive strength reduces by 50% and 45%,
respectively (Figure 5.4). This reduction in strength can be attributed to the reduced packing
of the materials as fly ash is fine powdered material which fills the voids created by stone dust
and later by pond ash. Also, the strength reduction is evident due to increase in initial porosity
of the system from 14.26% to 35.07% in case of fly ash replacement with pond ash (series B)
and from 14.26% to 29.26% in case of fly ash replacement with coal cinder (series C).

43
 Compressive strength (MPa) 9
8
7
6
5
4 3 Days
3 7 Days
2
14 Days
1
28 Days
0
56 Days

Series B-Replacement of fly ash with Series C-Replacement of fly ash with
pond ash coal cinder

Figure 5.4: Compressive strength (MPa) for replacement of fly ash from reference mix with
pond ash and coal cinder at different curing age

9.00
Compressive strength (MPa)

8.00
7.00
6.00
5.00 Series B
4.00
Series C
3.00
2.00
1.00
100% 80% 60% 40% 20% 0%
Percentage of Fly Ash (% )

Figure 5.5: Comparison of compressive strength (MPa) for replacement of fly ash with pond
ash and coal cinder in reference mix at curing age of 56 days

With the decrease in the percentage of fly ash, Figure 5.5 shows a higher reduction of strength
when the fly ash is replaced by pond ash (series B) compared to coal cinder blends (series C).
This can be attributed to the lower lime reactivity of pond ash compared to coal cinder. It is
interesting to note that coal cinder has highest lime reactivity value of 2.92. When the coal
cinder replaces fly ash from the reference mix, it should increase the compressive strength of
the blends but on contrary to that, it decreases the compressive strength due to its porous

44
structure resulting in increased porosity of the system. The compressive strength results for the
addition of paper sludge and marble dust are shown in Figure 5.6.

14
Compressive strength (MPa)

12
10
8
3 Days
6
7 Days
4
14 Days
2 28 Days
0 54 Days

Series D-Addition of paper sludge Series E-Addition of marble dust

Figure 5.6: Compressive strength (MPa) for addition of paper sludge and marble dust to the
reference mix at different curing age

It can be inferred from the results that there is a drastic reduction of compressive strength in
series D blends with the addition of paper sludge. This is attributed to the flaky and porous
structure of the paper sludge and due to the tendency to form lumps in the mix which in turn is
responsible for the very high initial porosity. While for the addition of marble dust,
compressive strength has significantly increased compared to the reference mix with the
highest compressive strength of 13.014 MPa, with a 10% marble dust addition at the age of 28
days. This remarkable improvement in the compressive strength can be accredited to the finer
particle size of marble dust, which resulted in a reduction in initial porosity of the blends from
14.26% to 5.91%. Although, there is further decrease in the initial porosity for 20% and 30%
addition of marble dust but there is no further improvement in the compressive strength. Figure
5.7 shows the variation of compressive strength for the addition of paper sludge (series D) and
marble dust (series E) at the age of 28 days. From the above-discussed results, it can be inferred
that compressive strength of the bricks decreases when the stone dust from is replaced with
pod ash. There is further decrease in the compressive strength with the replacement of fly ash
with pond ash and coal cinder respectively. Compressive strength is drastically reduced with
the addition of paper sludge to the bricks, but the addition of marble dust to the bricks
significantly increases the compressive strength of the bricks.
45
 15.0
Compressive strength (MPa) 13.5
12.0
10.5
9.0
7.5 Series D
6.0
4.5 Series E
3.0
1.5
0.0
0% 5% 10% 15% 20% 25% 30%
Addition of paper sludge & marble dust (%)

Figure 5.7: Comparison of compressive strength (MPa) for addition of paper sludge and
marble dust to the reference mix at curing age of 28 days
5.2.2 Relationship between ultrasonic pulse velocity, compressive strength, density and
water absorption
Ultrasonic pulse velocity (UPV) increases with an increase in the curing age of the specimen
for all the blends. Higher the UPV, higher should be the uniformity of the bricks. Figure 5.8
shows results for UPV at a different age for series A. UPV at the age of 56 days ranged from
2.82 to 2.20 km/s for series A. There is a decrease in the UPV of bricks with the replacement
of stone dust with pond ash at all the ages. This can be explained by a decrease in the stone
dust and increase in pond ash, which is increasing the porosity of the system.

3.0
Ultrasonic pulse velocity (km/s)

2.8
2.6
2.4
2.2 Base Mix (BM)
2.0 PA-12.5%
1.8 PA-25%
1.6
PA-37.5%
1.4
1.2 PA-50% (RM)
1.0
3 7 14 28 56
Curing Age (Days)

Figure 5.8: UPV (km/s) for series A blends at different curing age

UPV results for replacement of fly ash with pond ash and coal cinder are shown in Figure 5.9
and Figure 5.10.

46
 3.0
Ultrasonic pulse velocity (km/s)
2.8
2.6
2.4
2.2 PA-50% (RM)
2.0 PA-62.5%
1.8 PA-75%
1.6
PA-87.5%
1.4
1.2 PA-100%
1.0
3 7 14 28 56
Curing Age (Days)

Figure 5.9: UPV (km/s) for series B blends at different curing age
For series B there is a very small reduction in the UPV for first four blends but for complete
pond ash brick, there is a 16% reduction in the UPV from 2.20 to 1.86 km/s at the age of 56
days. This can be due to the complete replacement of fly ash with pond ash as fly ash has pore
refinement ability and is also responsible for the pozzolanic reaction. For series C, blends with
the replacement of fly ash from reference mix with coal cinder, steep reduction with every next
blend is observed. UPV reduced by 40% as compared to the reference mix. This is obvious as
coal cinder is highly porous material thus, even though the reactivity of coal cinder is higher
compared to fly ash, it causes reduction in the uniformity of the matrix.
For addition of paper sludge to the reference mix, the values of UPV are drastically reduced
compared to the reference mix which is shown in Figure 5.11. This is because of the flaky
structure of the particles of paper sludge and their tendency to agglomerate when mixed along
with water. It has been observed that paper sludge tends to form lumps in the brick specimens
which reduces the uniformity. Lowest UPV value of 0.58 km/s has been reported for the 30%
addition of paper sludge at the age of 56 days.
With the addition of marble dust to the in the reference mix, an improvement has been observed
in the UPV as shown in Figure 5.12. Marble dust is very fine and helps in further pore
refinement. It can also be related to the reduced initial porosity of the blends compared to
reference mix. The highest value of UPV (2.75 km/s) at the age of 28 days is reported for the
mix with 10% addition of marble dust.

47
 2.8
Ultrasonic pulse velocity (km/s)
2.6
2.4
2.2
2.0 PA-50% (RM)
1.8 CC-12.5%
1.6 CC-25%
1.4
CC-37.5%
1.2
1.0 CC-50%
0.8
3 7 14 28 56
Curing Age (Days)

Figure 5.10: UPV (km/s) for series C blends at different curing age

2.4
Ultrasonic pulse velocity (km/s)

2.2
2.0
1.8
1.6 PA-50% (RM)
1.4
1.2 PS-10%
1.0 PS-20%
0.8 PS-30%
0.6
0.4
3 7 14 28 56
Curing Age (Days)

Figure 5.11: UPV (km/s) for series D blends at different curing age

3.0
Ultrasonic Pulse Velocity (km/s)

2.8
2.6
2.4
2.2 PA-50% (RM)
2.0
1.8 MD-10%
1.6 MD-20%
1.4 MD-30%
1.2
1.0
3 7 14 28
Curing Age (Days)

Figure 5.12: UPV (km/s) for series E blends at different curing age

48
As per the observations shown in Figure 5.13, compressive strength is linearly correlated with
the ultrasonic pulse velocity. It can also be asserted that higher the compressive strength, higher
the UPV.

14.0
Compressive strength (MPa)

12.0
Series A
2.52
10.0
Series B
2.15
8.0
R² = 0.7104 1.50
Series C
6.0
0.85
Series D
4.0
Series E
2.75
2.0
0.0
0.00 0.50 1.00 1.50 2.00 2.50 3.00
Ultrasonic pulse velocity (km/s)

Figure 5.13: Relationship between compressive strength (MPa) and UPV (km/s) at the age of
28 days

Bulk density of bricks has a direct correlation with the UPV. Higher the UPV, higher will be
the density of bricks. Figure 5.14 shows the relationship between UPV and density of bricks.

1.80
1.60
1.40
Bulk density (g/cc)

R² = 0.8276 Series A
2.52
1.20
Series B
2.13
1.00
Series C
1.66
0.80
Series D
0.69
0.60
Series E
2.59
0.40
0.20
0.00
0.00 0.50 1.00 1.50 2.00 2.50 3.00
Ultrasonic pulse velocity (km/s)

Figure 5.14: Relationship between bulk density (g/cc) and UPV (km/s) at the age of 28 days

Water absorption and UPV are inversely proportional. Figure 5.15 shows the relationship
between water absorption and UPV at the age of 28 days. Higher the UPV, lower shall be the
water absorption of bricks.

49
 40.0%
35.0%
Water absorption (%)

30.0%
2.52
Series A
25.0% 2.06
Series B
R² = 0.8086
20.0% Series C
1.66
15.0% 0.85
Series D
10.0% 2.75
Series E
5.0%
0.0%
0.00 0.50 1.00 1.50 2.00 2.50 3.00
Ultrasonic pulse velocity (km/s)

Figure 5.15: Relationship between water absorption (%) and UPV (km/s) at the age of 28
days

5.2.3 Effect of industrial waste on water absorption and bulk density

Results for water absorption at 56 days ranges from 15.4% to 19.8% for series A. Base mix has
a water absorption of 15.4% and reference mix has a water absorption of 19.8%. An increase
of 28.5% is observed in the reference mix as compared to the base mix. The addition of pond
ash to the reference mix instead of fly ash results in an increase of 36% in the water absorption
compared to the reference mix. Pond ash is a water absorbent material that increased the water
absorption capacity of the hardened matrix.
When coal cinder is added to the reference mix instead of fly ash, it results in a 20% increase
in water absorption compared to the reference mix. Although coal cinder itself has a higher
water absorption but it reduces the overall water absorption capacity of the matrix due to its
finer particle size. Thus, in terms of water absorption coal cinder performs better as a
replacement of fly ash.
The addition of paper sludge to the reference mix results in significant increase in the values
of water absorption. For just 10% addition it increases the water absorption by 29% compared
to the reference mix. Further for 20% and 30% addition it raises the water absorption capacity
of reference mix by 44% and 77%, respectively. This can be explained as the paper sludge
itself has a very high water absorption (70% by weight). The addition of marble dust has a
positive effect on the water absorption values of reference mix. With 10% addition of marble
dust, the water absorption decreases from 19.8% to 15.4% (22% decrease compared to
reference mix) at the age of 28 days. For 20% and 30% addition, water absorption of reference

50
mix decreases by 11% and 29%. Thus, marble dust addition decreases the water absorption
capacity of the bricks. This can be attributed to a very fine particle size of marble dust particles
resulting in pore refinement of the matrix as its addition has decreased the initial porosity of
the blends.

14.0
Compressive strength (MPa)

12.0
20%
Series A
10.0
Series B
22%
8.0
20%
Series C
6.0
R² = 0.7521 25%
Series D
4.0
14%
Series E
2.0
0.0
0% 5% 10% 15% 20% 25% 30% 35% 40%
Water absorption (%)

Figure 5.16: Relationship between compressive strength and average water absorption at the
age of 28 days

It is obvious to state that, compressive strength is inversely proportional to the water

absorption. As the compressive strength of the matrix decreases, the percentage water
absorption increases. It is attributed to the fact that higher the compressive strength, lower is
the porosity of the matrix. It becomes evident from the Figure 5.16 that for all the blends from
series A to series E, water absorption capacity has increased with a decrease in the compressive
strength and vice versa.
The bulk density of brick specimens can directly be related to the specific gravity of the
constituent raw materials and their packing in the matrix. Bulk density can also be related to
the initial porosity of the matrix. The bulk density of the bricks is directly correlated with the
compressive strength of the bricks. It has been observed that higher the density of the brick,
higher is the compressive strength. Figure 5.17 depicts the relationship between the
compressive strength and density at the age of 28 days and also explains the effect of various
replacements and addition on the density of the brick. The base mix has the highest density of
1.69 gm/cc. This can be related to the use of stone dust in the blend, which is a heavy material
and has a specific gravity of 2.85. In series A, on replacement of stone dust with pond ash, the
reference mix has a density of 1.34 g/cc. Thus, the pond ash made the bricks 21% lighter
compared to the base mix. This is because of lower specific gravity of pond ash then the stone

51
dust. With further addition of pond ash in series B for replacement of fly ash, bricks became
16% lighter compared to the reference mix.

14.0
Compressive strength (MPa)

12.0
10.0 1.69
Series A
Series B
1.12
8.0
R² = 0.7676 1.25
Series C
6.0
1.17
Series D
4.0
1.53
Series E
2.0
0.0
0.80 0.90 1.00 1.10 1.20 1.30 1.40 1.50 1.60 1.70 1.80
Bulk density (g/cc)

Figure 5.17: Relationship between average bulk density and compressive strength for various
blends of series, at the age of 28 days

In series C, on a complete replacement of fly ash with coal cinder, the bricks became 18% light
compared to reference mix. As coal cinder is very light material (specific gravity, 1.26), it is
obvious to have a reduction in the density, but not much reduction is observed, which might be
due to the higher packing of material in the matrix.
With the addition of paper sludge a drastic reduction in the density has been observed. On 10%,
20%, and 30% addition of paper sludge, the density of the reference mix reduces by 13%, 22%,
and 37%, respectively. It has been observed that on 30% addition of paper sludge makes the
specimens float on water while testing them for water absorption. This reduction of density is
due to very low specific gravity of paper sludge and it tendency to agglomerate and form lumps
in the matrix which created voids.
The addition of marble dust increases the density of the bricks. With 10% addition, the density
of the reference mix increased by 14%. This can be attributed to the heavy mass of the marble
dust. With the further addition, the increase in the density is not significant as marble dust have
been reported to increase the packing of the matrix and fills the voids created by pond ash and
fly ash.
5.2.4 Efflorescence
Results for efflorescence was considerably rewarding and promising. The bricks developed in
this study showed no efflorescence for series A, B, C, and E. Slight efflorescence was detected
for series D brick specimens, as the white or grey deposits were less than 10%.

52
5.2.5 Effect of initial porosity on compressive strength, UPV, water absorption and bulk
density
Initial porosity of the blend can be a governing factor to control the compressive strength of
the bricks. With the replacement of stone dust from base mix the porosity increase from 3.29%
to 14.26% for reference mix. Stone dust has an angular particle, which improves the initial
porosity by interlocking. Initial porosity for series B and series C blends increased from 14.26%
to 35.07% and 29.26%, respectively. And for the addition of paper sludge increases the porosity
from 14.26% to 29.26% on 10% addition. This can be explained by the porous structure of
paper sludge and its tendency to form lumps in the matrix. The addition of marble dust has a
positive and rewarding effect on the initial porosity of reference mix. For 10% addition of
marble dust porosity of reference mix improves by 58% and with further addition it improves
the porosity by 72% and 89% for 20% and 30% addition, respectively. This improvement of
initial porosity can be attributed to the fine particle size of marble dust and its pore filling ability
thereby increasing the packing of the matrix. Compressive strength and UPV are directly
correlated with initial porosity in the bricks specimens. Lower the initial porosity, higher shall
be the compressive strength and UPV. Figure 5.18 and Figure 5.19 depicts the effect of initial
porosity of the mix on compressive strength and UPV of bricks at the age of 28 days.

14.0
Compressive strength (MPa)

12.0
3%
Series A
10.0
26%
Series B
8.0
17%
Series C
6.0
R² = 0.7850 30%
Series D
4.0
6%
Series E
2.0
0.0
0% 5% 10% 15% 20% 25% 30% 35% 40%
Initial porosity (%)

Figure 5.18: Effect of initial porosity on compressive strength of bricks at the age of 28 days
Figure 5.19 and Figure 5.21 depicts the relationship of initial porosity with water absorption
and bulk density. As the initial porosity of bricks increases, water absorption also increases.
Water absorption of brick is directly proportional with its initial porosity. While the bulk
density of the brick is inversely proportional with initial porosity. So, as the initial porosity
increased bulk density decreases.

53
 3.0

Ultrasonic pulse velocity (km/s)

2.7
2.4
3%
Series A
2.1
1.8 26%
Series B
1.5 29%
Series C
R² = 0.6507
1.2 36%
Series D
0.9
2%
Series E
0.6
0.3
0.0
0% 5% 10% 15% 20% 25% 30% 35% 40%
Initial porosity (%)

Figure 5.19: Effect of initial porosity on UPV of bricks at the age of 28 days

40.0%
35.0%
Water absorption (%)

30.0% Series A
3%
25.0% Series B
26%
R² = 0.8085
20.0% Series C
17%
15.0% Series D
30%
10.0% Series E
6%
5.0%
0.0%
0% 10% 20% 30% 40%
Initial porosity (%)

Figure 5.20: Effect of initial porosity on water absorption of bricks at the age of 28 days

2.0
1.8
1.6
Bulk density (g/cc)

1.4 3%
Series A
R² = 0.852
1.2 26%
Series B
1.0 17%
Series C
0.8
0.6 30%
Series D
0.4 Series E
6%
0.2
0.0
0% 10% 20% 30% 40%
Initial porosity (%)

Figure 5.21: Effect of initial porosity on bulk density of bricks at the age of 28 days

54
From the overall discussion in this chapter, we can suggest that initial porosity plays a pivotal
role in the compressive strength of bricks. It also affects the UPV, water absorption and bulk
density of bricks. Thus, initial porosity is a governing factor in the development of bricks
incorporating any new industrial waste.

55
 CHAPTER 6: SUMMARY & CONCLUSIONS

6.1 Summary
The study explored ways to safely and gainfully utilize various hazardous and non-hazardous
industrial waste by incorporating them in the production of non-structural, unfired bricks. It
provided the brick industry with several innovative raw materials such as paper sludge, pond
ash, coal cinder and marble dust for brick manufacturing and established a way to
examine/select or formulate an adequate feed mixture containing a new solid-waste material
for making unfired bricks.
Initially, all the collected industrial waste were characterized based on their physical and
chemical properties like specific gravity, loss on ignition, and water absorption. While the
specific surface area was determined using Blaine’s air permeability apparatus. XRD
characterization was carried out to determine various crystalline phases in the industrial waste.
Reactivity of raw materials was tested by measuring their lime reactivity and isothermal
calorimetry.
After successful characterization, mixture proportions for various blends were defined for the
casting of specimens. Optimized and commercially produced mix proportion by TARA was
used as a base mix, which consisted of ‘fly ash-stone dust-lime-gypsum’ system. Series A
attempted to utilize pond ash instead of stone dust and ‘fly ash-pond ash-lime-gypsum’ system
of brick manufacturing was developed termed as reference mix. Further study was carried out
to replace fly ash from the reference mix as fly ash has gained popularity as useful raw material
in various applications. Thus, with a view to replace fly ash from bricks with another industrial
waste like pond ash and coal cinder was attempted in series B and C blends. This resulted in
the development of ‘100% pond ash-lime-gypsum’ system and ‘coal cinder-pond ash-lime
gypsum’ system of production of non-structural unfired bricks. In order to utilize paper sludge
and marble dust in the bricks, the effect of their addition to the reference mix was evaluated. A
total of more than 900 odd brick specimen were cast in this study for 19 different blends. The
performance of newly developed bricks was evaluated based on various laboratory tests such
as compressive strength test, UPV test, water absorption, and efflorescence. Effect of factors
such as initial porosity of the mix was also studied.
This study paved a way to better understand the effect of incorporating various industrial waste
in the bricks and evaluate the performance of the newly developed unfired brick production
system.

56
6.2 Conclusions
The specific findings with respect to various unfired bricks production system developed in
this study lead to the following conclusions:
 Compressive strength and UPV decreases with increasing percentage replacement of stone
dust with pond ash. The compressive strength of ‘fly ash-pond ash-lime-gypsum’ system
reduces by 50% for complete replacement of stone dust with pond ash from the base mix.
There is an increase of 28.5% water absorption in the reference mix compared to the base
mix. The addition of pond ash instead of stone dust makes the brick 21% lighter compared
to the base mix. These results can be explained as pond ash is light weight and increases
the initial porosity of the system from 3.29% to 14.26%, and has a porous structure and
finer particle size compared to stone dust, which is a heavy coarser material and improves
packing of the matrix through interlocking.
 Compressive strength and UPV decreases with increasing percentage replacement of fly
ash from the reference mix with pond ash and coal cinder. ‘Coal cinder-pond ash-lime-
gypsum’ system has lower compressive strength reduction compared to ‘pond ash-lime-
gypsum’. This can be because of higher reactivity coal cinder compared to pond ash. The
addition of pond ash and coal cinder instead of fly ash results in an increase of 36% and
20% respective increase in the water absorption compared to the reference mix. Although
coal cinder itself has a higher water absorption but it reduces the overall water absorption
capacity of the matrix due to its finer particle size. Thus, in terms of water absorption coal
cinder performs better as a replacement of fly ash.
 On replacement of fly ash with pond ash and coal cinder, brick becomes 16% and 18%
lighter compared to the reference mix of ‘fly ash-pond ash-lime-gypsum’ system.
 The addition of paper sludge has a negative effect on the compressive strength, UPV, and
water absorption. For 10% addition, it decreases the compressive strength and UPV by 13%
and 59% respectively and increases the water absorption by 29% compared to the reference
mix. The addition of paper sludge has a drastic reduction in the density of the bricks. This
is attributed to the flaky and porous structure of the paper sludge and its tendency to form
lumps in the mix which in turn is responsible for the very high initial porosity.
 While the addition of marble dust increases the compressive strength and UPV. Marble
dust blends with 10% addition reports the highest compressive strength of 13.014 MPa and
UPV of 2.75 km/s at the age of 28 days. It also improves the water absorption by 22%. This
remarkable improvement in the compressive strength can be accredited to the finer particle

57
 size of marble dust, which reduces the initial porosity of the blend from 14.26% to 5.91%
by improving the packing of constituent materials.
 The addition of marble dust increases the density of the bricks. With 10% addition, the
density of the reference mix increased by 14%. This can be attributed to the heavy mass of
the marble dust. With the further addition, the increase in the density is not significant as
marble dust have been reported to increase the packing of the matrix and fills the voids
created by pond ash and fly ash.
 There is a substantial increase in the compressive strength from 28 days to 56 days of curing
age.
 UPV increases with increase in the curing age of brick specimen for all the blends.
 The compressive strength of bricks is linearly correlated with the ultrasonic pulse velocity.
It can also be asserted that higher the compressive strength, higher the UPV.
 The compressive strength of bricks is inversely proportional to the water absorption. As the
compressive strength of the matrix decreases, the percentage water absorption increases. It
is attributed to the fact that higher the compressive strength, lower is the porosity of the
matrix.
 The bulk density of brick specimens is directly related to the specific gravity of the
constituent raw materials and their packing in the matrix. Bulk density can also be related
to the initial porosity of the matrix. The bulk density of the bricks is directly correlated with
the compressive strength of the bricks. It has been observed that higher the density of the
brick, higher is the compressive strength.
 Initial porosity of the blend is one of the governing factor which controls the compressive
strength, UPV and water absorption of the bricks. As the initial porosity increases,
compressive strength and UPV decreases and water absorption increases.
 Based on the result and analysis of this study, it is possible to correlate and predict the
approximate compressive strength of bricks, based on the initial porosity of the matrix.
 Comparative compressive strength for various design mix blends used in this study are
listed in Table 6.1.
The results of this study indicate that bricks that contained industrial waste like pond ash, coal
cinder, and marble dust had marketable properties as controlled low strength, non-structural
unfired bricks. The result of this study also provides the brick industry with readily available
new raw materials for brick making and the waste generating industry with possible cost-saving
advantage by reducing or eliminating their waste disposal.

58
 Table 6.1: Comparative compressive strength for various bricks blend used in this study

Compressive
Bricks
strength

Base mix ('Fly ash-stone dust-lime-gypsum' system) Good

Replacement of stone dust with pond ash ('Fly ash-pond ash-lime-

Reduced, Good
gypsum' system) Reference mix
Replacement of fly ash with pond ash ('Fly ash-pond ash-lime-gypsum'
Reduced, Poor
system)
Replacement of fly ash with coal cinder ('Coal cinder-pond ash-lime-
Better
gypsum' system)
Addition of paper sludge ('Fly ash-pond ash-paper sludge-lime-gypsum' Highly reduced
system) (Poor)
Addition of marble dust ('Fly ash-pond ash-marble dust-lime-gypsum'
Best
system)

The bricks developed in this study are eco-friendly and can be marketed as sustainable
construction material.

6.3 Future perspectives

The results embedded in this present work and analysis of the experimental data suggests
carrying out following work:
 XRD and XRF analysis of the samples to study detailed phase formation behaviour.
 Identification of other process variables like initial porosity and their effect on properties
of bricks in order to develop a Mix-Design methodology for commercially producing
bricks.
 Optimization of other process parameters like curing condition, temperature, forming
pressure etc. by further carrying out experimental work.
 Study and testing the durability properties of bricks developed in this study.
 Study the thermal conductivity properties of bricks developed.
 Synthesis of full-scale samples to conduct the in-situ test.
 Study the economic feasibility and life-cycle assessment of brick produced, for commercial
production.

59
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