THESIS: POTENTIAL APPLICATION OF RECYCLED GARNET AS POZZOLAN

MATERIAL IN CONCRETE

MUHAMMAD NAZIM BIN AHMAD

55214114010

Report Submitted to Fulfil the Partial Requirements for the Bachelor of

Chemical Engineering Technology (Hons.) in Environment
Universiti Kuala Lumpur

August 2017

ii
 DECLARATION

I declare that this thesis entitled “Potential Application of Recycled Garnet as

Pozzolan Material in Concrete” is the result of my own research and my
original work and all references have been cited adequately as required by
the University.

Date: Signature:
(Hardcover submission date) Full Name: MUHAMMAD NAZIM BIN
AHMAD
ID Number: 55214114010

I
 APPROVAL PAGE

We had supervised and examined this report and verify that it meets the
program and University’s requirement for the Bachelor of Chemical Engineering
Technology (Hons.) in Environment.

Date: Signature:
(Hardcover submission date) Supervisor: Dr. Amelia Md Som
Official Stamp:

II
 ACKNOLEDGMENT

Grateful appreciation in the presence of Allah for His grant and guidance that
finally I manage to finish my final year project. I would like to express my
biggest gratitude to my project supervisor, Dr. Amelia Md Som for providing
essential guidance, motivation, direction and encouragement during my
research. I would also like to express my gratitude to UniKL MICET
technicians, Mr Mohd Aizuddin Shahmi bin A’zim and Mr Hairool Hisham bin
Roslan for giving guidance to use equipment to perform better analysis. My
biggest thank you to my parents who continuously provide me strength and
advice. I am extremely grateful for their assistance and suggestions throughout
my project. The completion of this thesis would not be possible without all of
them.

III
 CONTENTS

DECLARATION I

APPROVAL PAGE II

ACKNOLEDGMENT III

LIST OF TABLES IV

LIST OF FIGURES IV

ABSTRACT V

ABSTRAK VI

CHAPTER 1: INTRODUCTION 7

1.0 Introduction 7
1.1 Problem Statement 8
1.2 Objective 8
1.2.1 General objective 8
1.2.2 Specific Objectives 9
CHAPTER 2: LITERATURE REVIEW 10

2.1 Portland cement 10

2.1.1 History of Portland cement 10
2.1.2 What is Portland cement 10
2.2 Pozzolan 10
2.2.1 What is pozzolan 10
2.2.2 Type of Pozzolan 10
2.2.3 Pozzolan used as supplementary cementitious materials 11
2.2.4 Reaction in cement 11
2.2.5 CSH 11
2.2.6 Abrasive blasting 11
2.2.7 Garnet 12

1
 2.2.8 Recycle garnet 12
2.2.9 Garnet as pozzolan material in concrete 12
2.3 Hydration 12
2.3.1 Hydration reaction 12
2.3.2 Methanol as a reagent to stop hydration reaction 12
2.4 The durability criteria of mortar 13
2.4.1 Compressive strength of mortar 13
2.4.2 Density of the Garnet R mortar 13
2.4.3 Carbonation of Garnet R mortar samples 14
2.4.4 pH value of Garnet R mortar 14
2.4.5 Moisture content 15
2.4.6 Water absorption 15
2.4.7 Thermogravimetric analysis 15
CHAPTER 3: RESEARCH METHODOLOGY 16

3.0 Research Methodology 16

3.1 Preparation of mould sample: 16
3.2 Preparation of control sample 17
3.2.1 Preparation of control sample 17
3.2.2 Mortar paste compaction 17
3.3 Garnet R mortar paste preparation for 10%, 20% and 30% samples 18
3.3.1 Sample curing age 18
3.4 Test Analysis 18
3.4.1 Compressive strength testing 18
3.4.2 Carbonation test 19
3.4.3 pH test 20
3.4.4 Moisture content Test 20
3.4.6 Thermogravimetric Analysis (TGA) 20
3.4.7 Water Absorption test 20
CHAPTER 4: RESULT AND DISCUSSION 22

4.1 Analysis for Garnet R mortar 22

4.2 Compressive strength of mortar 22
4.3 Density 24
4.4 Carbonation 25
4.5 pH test 28
4.6 Moisture content test 29
4.7 Water Absorption 30
4.8 Thermogravimetric Analysis 31

2
CHAPTER 5: CONCLUSION AND RECOMMENDATION 34

5.1 Conclusion 34
5.2 Recommendation 34
REFERENCES 35

3
 LIST OF TABLES

Table 3.1 The formulation of Cement-Garnet mortar sample with 14

control sample for 28 days of curing time
Table 4.1 Comparability of Strength Activity Index (SAI) of ASTM 19
and analysis result
Table 4.2 Phenolphthalein Test on mortar 24

LIST OF FIGURES

Figure 3.1 Moulds preparation from PVC of 100mm height and 50 mm 13

diameter 13
Figure 3.2 Compressive strength machine 16
Figure 4.1 Compressive strength of Garnet R mortars for 28 days
and 73 days (error bar represents Standard Deviation) 20
Figure 4.2 Slanting surface of the mortar before compressive strength
test 21
Figure 4.3 Measured density of 28 days curing mortars (error bar
represents Standard Deviation) 22
Figure 4.4 pH of mortar (28 days curing) (error bar represents
Standard Deviation) 26
Figure 4.5 Moisture content of mortar samples of 28 days curing
(error bar represents Standard Deviation) 27
Figure 4.6 Water absorption of Garnet R mortar (error bar
represents Standard Deviation) 28
Figure 4.7 TGA graph for 10% Garnet R sample 30
Figure 4.8 TGA graph for 20% Garnet R sample 30
Figure 4.9 TGA graph for 30% Garnet R sample 31

IV
 ABSTRACT

This article summarizes the application of recycled garnet (Garnet R) as pozzolan to partially replace
the cement inclusion in a mortar to reduce carbon dioxide (CO2) emissions worldwide. The research
was conducted by preparing different percentages of Garnet R mortar at 0%, 10%, 20% and 30%.
The cement paste and mortar were prepared according to American Society for Testing Materials
(ASTM). Garnet R mortar was investigated by performing analysis of compressive strength, density,
carbonation, pH, moisture content, water absorption and Thermogravimetric analysis (TGA). Most
of the analysis was conducted under ASTM except water absorption which follows British Institution
Standard (BSI) due to limited equipment to test under ASTM. The result obtained shows some
fluctuation of data presented due to slanting surface at 20% of Garnet R. However, it was found that
durability of mortar is mostly dependable to compressive strength. The best compressive strength
obtained at 10% compared to 20% and 30% Garnet R mortar where pH value is the highest and
contain the lowest moisture content. Higher pH prevents corrosion attack which contradictory with
actual standard pH of mortar which is 9 while lower moisture content strengthens the mortar. The
best density observed was at sample 30% compared to 10% and 20% of Garnet R. Carbonation
test conducted which most of the samples has carbonated area. Water absorption obtained shows
that the sample of 20% Garnet R has the highest value compared to other samples which explain
the weak structure of mortar. TGA test graph shows that hydration, decomposition of portlandite
and carbonation reaction observed which has been discussed thoroughly. Thus, the research
proves that Garnet R can act as pozzolan in a mortar.

V
 ABSTRAK

Artikel ini merangkumi penggunaan garnet kitar semula (Garnet R) sebagai pozzolan untuk
menggantikan simen secara separa ke dalam mortar untuk mengurangkan pelepasan karbon
dioksida (CO2) di seluruh dunia. Kajian ini dijalankan dengan menyediakan peratusan yang berbeza
dari Garnet R mortar pada 0%, 10%, 20% dan 30%. Campuran simen dan mortar disediakan
mengikut American Society for Materials Testing (ASTM). Garnet R mortar dikaji dengan melakukan
analisis kekuatan mampatan, kepadatan, karbonasi, pH, kandungan lembapan, penyerapan air dan
analisis Thermogravimetric (TGA). Kebanyakan analisis dijalankan di bawah ASTM kecuali
penyerapan air yang mengikuti Standard Institusi British (BSI) disebabkan peralatan terhad untuk
diuji di bawah ASTM. Keputusan yang diperoleh menunjukkan beberapa turun naik data yang
dikemukakan disebabkan oleh permukaan yang condong pada 20% daripada Garnet R. Walau
bagaimanapun, didapati bahawa ketahanan mortar kebanyakannya bergantung kepada kekuatan
mampatan. Kekuatan mampatan terbaik diperoleh pada 10% berbanding 20% dan 30% Garnet R
mortar di mana nilai pH adalah yang tertinggi dan mengandungi kandungan lembapan yang paling
rendah. pH yang lebih tinggi menghalang serangan kakisan, bercanggah dengan piawai pH mortar
sebenar iaitu pH 9 manakala kandungan lembapan yang lebih rendah menguatkan mortar.
Ketumpatan terbaik yang diperhatikan adalah pada sampel 30% berbanding dengan 10% dan 20%
ujian Garnet R. Karbonasi yang mana kebanyakan sampel mempunyai kawasan berkarbonat.
Penyerapan air yang diperolehi menunjukkan bahawa sampel 20% Garnet R mempunyai nilai
tertinggi berbanding dengan sampel lain yang menjelaskan struktur lemah mortar. Grafik ujian TGA
menunjukkan bahawa penghidratan, penguraian reaksi portlandit dan karbonasi diperhatikan yang
telah dibincangkan dengan teliti. Oleh itu, penyelidikan membuktikan bahawa Garnet R boleh
bertindak sebagai pozzolan dalam mortar.

VI
 CHAPTER 1: INTRODUCTION

1.0 Introduction

Mortar is made up from cement, water and lime. The basic strength of concrete is depending on
water/cement ratio and become stronger over time as it can change it state from semi- fluid to fully-
cured solid. When these elements are mix together, it triggers a chemical reaction which called as
hydration reaction of cement. Thus, a gel formed which cover and fills the spaces between
aggregate which then harden into concrete. Mortar is mainly used in masonry construction, often
used to hold together different building materials such as brick, block or stones.
As the Portland cement hugely contribute to carbon dioxide emission worldwide, lot of
research done on pozzolan as supplementary cementitious material (SCM) to partly substitute the
cement to reduce the cement production. The characteristic of pozzolan that contribute to strong
structure, minimize the permeability of concrete resulting high durability of the concrete against
corrosion, acid attack and sulphuric attack. Pozzolan is defined as siliceous material which contain
little cementing properties, but will finely distribute form in the presence of moisture where it
chemically reacts with calcium hydroxide to form compounds possessing cementitious properties.
Pozzolan can be classified into artificial and natural. Artificial pozzolan is produced from human
activities such as fly ash and silica fume produce from by-product of burning pulverized coal in an
electrical generating station and by-product of producing silicon metal or ferrosilicon alloys. Natural
pozzolan such as kaolin and shale are form naturally where kaolin found in clay state and shale can
be found in sedimentary rocks state.
Garnet can be found in metamorphic and igneous rocks where it is formed under very high
temperature and pressure. The nation which usually be founded is Africa, India, Russia, United
States, Madagascar and Pakistan. Garnet is the material used in sand blasting which make the
rough surface smooth. The high abrasive characteristic of garnet gives the higher usage of this
natural resources where it can be used up to 5 times as abrasive material. The recycle garnet usually
in smoother powder form. The more it used the smoother the garnet. The idea of using recycled

7
garnet, Garnet R is to maximise the garnet waste from industrial and to minimise the cement usage.
This can contribute to more environmental friendly as less mining of abrasive garnet, lower the
cement production and reduce the dust form from the cement. The recycle garnet is used to
determine whether it has properties of hardened concrete or not. The recycle garnet still contain
siliceous material even though it has been used several times. The hardened factor of cement
basically siliceous component contains in recycle garnet where it chemical reaction occur.

Cement is form from clinker. It can be found widely used in the world. Cement usually contain
silicon oxide, calcium oxide, aluminium oxide and ferric oxide. This oxide component used to
determine the cementitious compound such as C3S, C2S, C3A and C4AF which have characteristics
in formation of concrete. Tricalcium silicate rapidly hardens the concrete which give the early
strength of the concrete, where the strength become higher if the percentage of C 3S in concrete is
higher.

1.1 Problem Statement

Around 7 % of global carbon dioxide emission is produce from cement industry. That is a huge
amount of carbon emission from single industry. By estimation, the cement production will arise from
2.55 billion ton in 2006 to 3.7-4.4 billion tons by 2050. This mean the carbon footprint also will
increase by 2050. Measures to reduce atmospheric carbon dioxide include energy conservation,
use of non-fossil fuel based energy sources, and carbon dioxide capture and storage (Iyer et al.,
2017).

To reduce carbon footprint, we want to test recycled garnet in concrete production by mixing
it with cement in different ratio. Some study has been done in mixing cement material such as
Magnesia, lime mortars, fly ashes and carbonated brine which proves the carbon emission
reduction. The production of cement need to be reduced so that the carbon footprint also can be
reduced.

1.2 Objective
1.2.1 General objective

The general objective of this research is to evaluate the potential of using Recycle Garnet (Garnet
R) in mortar without impacting the performance of the finished product.

8
1.2.2 Specific Objectives

The specific objectives of this research are:

1. To study the effect of different amount of Garnet R (10, 20 and 30%) on the compressive
strength of 28-day mortar and
2. To study the effect of different amount of Garnet R (10, 20 and 30%) on the cement hydration
process by using thermogravimetric (TGA)
3. To study the effect of different amount of Garnet R on the pH value of the mortar
4. To study the water absorption of mortar with Garnet R.
5. To study the resistance and durability of mortar from corrosion through by using Carbonation
test.

9
 CHAPTER 2: LITERATURE REVIEW

2.1 Portland cement

2.1.1 History of Portland cement

Portland cement has been discovered and used by Roman empire. History suggests that the Ancient
Romans were the first to widely use a material that had any connection to modern concrete in their
constructions (Strenchock, 2009).

2.1.2 What is Portland cement

Portland cement is the material that has adhesive and cohesive properties which enable it to attach
minerals fragments into a solid structure such as bricks, stone and sand (Salah, 1995). Portland
cement is mixed with sand, rushed rock and water to produce concrete which most widely used in
construction material (Mehta et al., 2006).

2.2 Pozzolan
2.2.1 What is pozzolan

Pozzolan is described as a material that can hardened concrete whether through hydraulic or
pozzolanic activity or both when used in Portland cement. (Halit, 2011). Al-chaar et al. (2013) define
pozzolan as inexpensive siliceous material to substitute for cement in mortar mixtures.

2.2.2 Type of Pozzolan

Pozzolan can be divided into two types, natural and artificial. Halit (2011) stated that the source of
natural pozzolan such as volcanic ash, volcanic tuff and pumicate while the source of artificial such
as fly ash, silica-fume and granulated blast furnace slag.

10
2.2.3 Pozzolan used as supplementary cementitious materials

Pozzolan is supplementary cementitious materials (SCM) which contribute to better strength and
durability of concrete. It has been proved by many research that additional of pozzolan in concrete
paste increase the strength of concrete. One of the research is done by Amin et al. (2012). They
stated that the object of producing pozzolan cements has been of considerable scientific and
technological interest because such addition of pozzolan increases the chemical resistance to
sulphate attack, inter-permeability, lowering heat of hydration, and thermal expansion. SCM’s may
produce hydraulic and pozzolanic reactions. The first ones are chemical reactions due to hydration
that enable hardening which is a similar reaction to that of Portland cement López et al. (2010).

2.2.4 Reaction in cement

When water and cement are mixed together, two chemical reaction occur which is hydration and
pozzolanic reaction. Hydration reaction is a hardening process of concrete which is similar reaction
to that of Portland cement. (Halit, 2011). Pozzolanic reaction occurred when in the presence of
water, calcium hydroxide (CaOH also known as portlandite) reacts to produce calcium silicate
hydrates (C-S-H) López et al. (2010). Below is the pozzolanic reaction:

Calcium Hydroxide + Silica + Water  Calcium Silicate Hydrate + Calcium Hydrate

2.2.5 CSH

Calcium silicate hydrates through pozzolanic reaction contributes to concrete microstructure

densification, to decrease porosity and to increase strength (López et al., 2010). Halit (2011)
mentioned that CSH contain hydraulic binding property which support the structure of concrete
material.

2.2.6 Abrasive blasting

Abrasive blasting is a method used to clean up surfaces from contaminants and provide new rough
surface for new coating (Kambham et al., 2007). This statement also supported by Byrne et al.,
(2013) where abrasive blasting proven to remove metal oxide and roughen the surface.

11
2.2.7 Garnet

Garnet is a crystalline rocks mineral of the Earth’s outer wall and lower surface layer and sometimes
occurs in volcanic liquids (Wood et al., 2013). He also stated that garnet has high density, low
compressibility and stability will increase as the pressure increase. Garnet can be used in wide
range of environments and one of the highest quality minerals in the earth, such as sedimentary
material and industry applications (Baxter et al., 2013).

2.2.8 Recycle garnet

Recycle garnet used is waste from industrial activities. So far, there is no specific study on the
recycle garnet as pozzolan in cement concrete. There are some similarities of recycle garnet with
other pozzolan used in formation of concrete which is it contains silica compound and available in
powder form.

2.2.9 Garnet as pozzolan material in concrete

The Garnet R is used as pozzolan material in this study. The additional of Garnet R may change
the hydration reaction rate in cement. This statement is supported by Gabrovšek, Vuk, & Kaučič
(2006) as they stated that the present of limestone as pozzolan material in cement will changes the
rate and degree of hydration change, as well as the composition of the hydrated cement paste.

2.3 Hydration
2.3.1 Hydration reaction

The reaction that occur in during the formation of concrete is hydration reaction. This reaction show
the changes of phases of cement in concrete. Pane & Hansen (2005) said the hydration,
representing mass conversion of different phases in the cement paste, ties closely to the
microstructure of concrete, which in turn relates to important physical properties such as strength,
elastic moduli, toughness, diffusivity and permeability. Thermogravimetric analysis (TGA) can also
determine the hydration reaction of concrete. Gabrovšek et al., (2006) use TGA in their study on
various carbonates for 7 and 28 days curing age concrete which represented in TGA/DTG graph.

2.3.2 Methanol as a reagent to stop hydration reaction

During the cementation, there is chemical reaction occurred called as hydration reaction. To cease
the reaction, the sample will be soaked with methanol. To stop hydration, exchange water, and
12
prevent carbonation, the samples were soaked in methanol and stored for 1 week (Pane & Hansen,
2005). But, other reagent such as ethanol can be used to stop hydration reaction. A study from
Gabrovšek et al., (2006) used ethanol and diethyl ether to stop the reaction of the hydrated samples
and dried overnight in a forced-air oven at 40 °C.

2.4 The durability criteria of mortar

2.4.1 Compressive strength of mortar

The compressive strength test is a very crucial aspect in mortar workability as it determines the
durability of the mortar. An article by National Ready Mixed Concrete Association (NRMCA, 2003)
stated that compressive strength provide vast range of mechanical and durability properties to meet
the design specifications of a structure. Two aspects of compressive strength determination
observed in this research; pozzolan as a replacement of cement and curing age. A study towards
metakaolin mortar and fly ash concrete by Siddique et al., (2009) and Siddique et al., (2011) as
pozzolan replacing cement in mortar obtain that the compressive strength increase as the
percentage of metakaolin and fly ash inclusion increase. Another research by Kanning et al., (2014)
on banana leaves ash (BLA) found that compressive strength increase at 5% BLA replacement, and
reach constant value at 7.5% and 10% BLA replacement. The compressive strength obtain were
inconsistent as the increasing in percentage of Garnet R replacement of cement in mortar. Hossain
et al., (2016) found that the compressive strength decreasing as the percentage replacement of
black rice husk ash (BRHA) increased. Conversely, BLA mortar has slow yet steady increase in
compressive strength as the curing age of mortar increase (Kanning et al., 2014).

2.4.2 Density of the Garnet R mortar

Density of mortar can affect the mortar compressive strength. High density indicates a higher
strength of mortar. Holm et al,. (2007) tested that high quality concretes can maintain low density
by limitedly absorbing water. They added that the concrete will lower in density due to moisture loss
where it corresponds to the ambient conditions and surface area/volume ratio of the concrete.
Carolina (2016) adding that as the curing age of concrete increases, the strength and density also
increase and reduces the absorption capacity. Raheem et al., (2013) explained that with proper
curing method, the significance value of density and compressive strength of concrete will be
achieved.

13
2.4.3 Carbonation of Garnet R mortar samples

To prevent corrosion in concrete, carbonation test essentially done to determine whether the
concrete able to withstand with environment that contain high carbon dioxide such as urban area.
Borges et al., (2010) mentioned that carbonation is a common problem faced by cement paste and
concrete. By spraying phenolphthalein to the surface of the mortar, the change of colour can be
observed. Gruyaert et al., (2013) stated that carbonated area are purple coloured while
uncarbonated area will colourless. Torgal et al., (2012) stated that at the uncarbonated area, the
specimen will change in colour to purple-red colour and no colouration occur at the carbonated area.
They also found that uncarbonated area has higher alkalinity, while the carbonated area has lower
alkalinity. The purple colour surrounds the surface of mortar indicate the area which carbonation
occurs. (Pacheco et al., 2012).The carbonation occurred almost at the outer surface of Garnet R
mortar samples.
This phenomenon occurs might be from several factors such as water binder ratio, porosity,
and permeability of the concrete (Hossain et al., 2016). In addition, Silva et al., (2015) proposed that
the rate of carbonation depends on the permeability, moisture content and relative humidity of the
concrete.
Peter et al., (2008) studied that the carbon dioxide is in an aqueous state will react with
calcium hydroxide, Ca(OH)2 during carbonation reaction to produce calcium trisilicate, CaSiO3. The
carbonation reaction also produces C-S-H as a product. The formation of CaCO3 will change the
porosity of the concrete as mentioned by Peter et al., (2008). Sisomphon & Franke (2007)
highlighted that chemical reaction occurs in carbonated area of concrete where cement hydration
product such as Ca(OH)2, react with carbon dioxide present in the atmosphere.

2.4.4 pH value of Garnet R mortar

High in pH value indicate that the carbonation will less likely occur in the mortar. Hence, chloride
attack can be prevented and make the Garnet R mortar to last longer than normal mortar. Rahman
(2014) stated that concrete with low quality usually has pH lower than 9. Contrary from mortar, pH
value lower than 9 will give the better durability of structure. Besides, Dong et al., (2014) studied
that pH can be affected by carbonation where it lowers the pH value. From the carbonation test, it
shows that Garnet R mortar samples are not affected by carbonation which have higher pH value.

14
2.4.5 Moisture content

A. Gardiner and K. MacDonald (2013) mentioned that moisture content is important criteria as it
influence the durability of the concrete. Costigan et al., (2014) stated that mortar with excessive
water content has low mechanical strength and the risk of cracking by shrinkage will be higher. High
moisture content will make the mortar weak as referred to the compressive strength at sample of
20% Garnet R.

2.4.6 Water absorption

Water absorption also part of durability of mortar. Poon et al., (2004) identify that strength
characteristics of concrete is influence by water absorption. Kannan et al., (2012) found that water
absorption of rice husk and metakaolin mortar were lower than ordinary cement mortar. With the
presence of pozzolan, the water absorption become lower as it blocks the pores inside the mortar.
Zhang et al., (2014) clarified that higher water absorption occurs at concrete with most porosity. The
water absorption of Garnet R mortar samples has fluctuated result where the water absorption
increases from 10% to 20% Garnet R inclusion and greatly drop at 30% of Garnet inclusion.
Gingos et al., (2011) studied on the pulverized fly ash (PFA) mortar and obtain higher water
absorption at 10% mixture, following declination in 20% and increase slightly at 30% admixture. A
similarly by Siddique et al., (2009), where they found that water absorption of metakaolin mortar
increase from 10% to 15% of metakaolin replacement, and decrease slightly at 20% of metakaolin
inclusion. Contrary with other studies, Dhinakaran & Chandana (2016) test the water absorption on
bamboo leaf ash (BFA) mortar and found that the water absorption increases as the percentage of
BFA increase from 10%, 20% and 30%.
This indicate that different type of pozzolan can influence the water absorption differently. It
can be deduced that the higher the water absorption, the lower the durability of mortar.

2.4.7 Thermogravimetric analysis

To determine the carbonation and hydration reaction occurred in mortar, thermogravimetric analysis
(TGA) was performed. Gabrovšek et al., (2006), Song et al., (2014) and Bernal et al., (2017) use
TGA to perform analysis on hydration reaction of mortar, and determine the carbonation depth of
the mortar by extracting data from the TGA graph.

15
 CHAPTER 3: RESEARCH METHODOLOGY

.
3.0 Research Methodology

In this chapter, the methodology used for preparation of mould and samples will be explain as well
as how the test was conducted during research.

3.1 Preparation of mould sample:

The preparation of cement paste and curing specimens is according to ASTM C 31/C 31M – 03a.

Figure 3.1 Moulds preparation from PVC of 100mm height and 50 mm diameter

The preparation of moulds is shown in Figure 3.1. A polyvinyl chloride (PVC) of 400mm of height
and 50mm of diameter were cut into four compartments by using PVC saw. Each compartment was
cut into 100 mm of height and 50 mm in diameter. After that, each 100mm PVC was cut in half to
16
ease the detachment of mortar from the mould. Finally, the half-cut PVC were tied by using black
tape to get the original and solid form of mould.

3.2 Preparation of control sample

The mortar proportion was tabulated in Table 3.1. The water-cement ratio used for the mixture is
0.45.

Table 3.1 The formulation of Cement-Garnet mortar sample with control sample for 28 days of
curing time
Combination
Curing C1 C2 C3 C4
time % Cement % Cement: Garnet
100 90:10 80:20 70:30
600g of 540g of Cement 480g of Cement 420g of Cement +
28 Cement + + 60g of Garnet + 120g of 180g of Garnet R
days 270mL of water R + 270mL of Garnet R + + 270mL of water
water 270mL of water

3.2.1 Preparation of control sample

A dry ingredient such as cement and garnet were prepared. The samples consist of 4 different
mixture which is 0%, 10%, 20% and 30% of Garnet R inclusion, with 3 replicate for each sample.
The cement mortar prepared was 12 in total. The basic mixture for the control sample, (0% Garnet
R) is water and cement. For the test samples, the amount of Garnet R, cement and water is mixed
differently in each mould according to the Table 3.1. For control samples, weight 600g of cement.
Add weighed cement into the mixing container. Add deionized water of 270 mL into the container.
Mix the cement with the deionized water properly until it changes state to semi-solid.

3.2.2 Mortar paste compaction

The prepared cement paste for each mixture was poured into the mould with approximately 3 equal
layers. In each layer, in constant manner, a tamping rod is used by compacting circularly for 25
times. For the first layer, the cement paste was poured 1/3 of the mould. The tamping rod was
ensured to not to touch the bottom of the mould during compacting. For the second and third layer

17
of mortar paste, the tamping rod was inserted approximately touch the previous top layer. The
excessive layer of cement was removed from the mould by using the tamping rod.

3.3 Garnet R mortar paste preparation for 10%, 20% and 30% samples

Cement and Garnet R was weighed by using weight balance. Approximately, cement and Garnet R
was weighted for 540g, 480g, 420g and 60g, 120g, 180g of the test sample of 10%, 20% and 30%
Garnet R according to Table 3.1. Since water to cement ratio is constant, approximately 270 mL of
deionized water was added to mixture container subsequently. Immediately mix the dry ingredient
after deionized water was poured until it becomes semi-solid. Let the mortar solidify for 24 hours at
room temperature.

3.3.1 Sample curing age

After 24 hours, the mould from each sample was removed, and soaked in a container with deionized
water. The samples were cured for 28 days. Each sample was taken out after 28 days and soaked
with methanol to intermediate the chemical or hydration reaction in mortar.

3.4 Test Analysis

There are 7 tests performed on the Garnet R mortar to determine the Garnet R as pozzolan to partly
replace the cement in the mortar. Each of the analysis is referred to the ASTM standard and BSI
standard.

3.4.1 Compressive strength testing

This test will be conducted based on ASTM C109. The compressive strength testing is conducted
after 28 days of curing. The specimen tested including control specimen (0%) and another specimen
with 10%, 20%, 30 % of a garnet mortar specimen. Before conducting the test, diameter and height
were measured by Vernier calliper while weight balance was used to measure the mortar mass.

18
 Figure 3.2 Compressive strength machine

Compressive strength machine, as shown in Figure 3.2 used to measure the strength of the mortar.
Compressive strength was recorded after the test done.

3.4.2 Carbonation test

The procedure of carbonation is started with the preparation of phenolphthalein solution. The mortar
sample from compressive strength were used for this test. The mortars were already in a split state
where phenolphthalein was sprayed onto the surface of mortar. Spray the phenolphthalein on the
split surface of the concrete of the concrete cylinder (Lo, 2005). The change in colour of split surface
mortar observed where it changes from grey into pink colour. The change of colour surface area
was observed to differentiate between carbonated and uncarbonated area, then captured by a
camera to represent as a data.

19
3.4.3 pH test

The pH meter needs to be calibrated at the beginning of the test. Buffer solution were used to
calibrate the pH meter so that the reading will be more accurate. Approximately 25g of mortar
samples was soaked in water before tested. Mix and stir the concrete powder with the 10mL of
distilled water at temperature of 22 ±1℃ (Grubb, Limaye, & Kakade, 2007). By inserting the pH
probe into the mixture, the reading of pH was recorded.

3.4.4 Moisture content Test

Moisture content test was conducted according to the ASTM D 2216-98. The initial mass of each
mortar was measured. Then, the mortars were placed in the 110 ±5℃ oven for 16 hours. The
mortars were taken out from the ovens and cooled down until it can be handled comfortably with
bare hands. The dried weight (final mass) of the mortars were measured. Then, the moisture content
of the mortars was calculated. Below is the formula used to calculate moisture content:

Moisture content= (weight Initial- weight after)/ (Wt. after - Wt. container) x 100

3.4.6 Thermogravimetric Analysis (TGA)

Thermogravimetric analysis was conducted by the technician. But the samples need to be prepared
first. The mortar fragment from compressive strength test was used by smashing it into tiny pieces.
Then, weight the mortar pieces up to approximately 10-20 mg. The required heating rate used is at
10℃ per minutes from 21 to 1100℃. The test was conducted for approximately 6 hours each sample
according to the technician in charge. After the test, 6 graphs obtain which is 0%, 10%, 20%, 30%
of Garnet R, TGA/DSC and TGA/DTG. The mass loss was observed to determine which peak the
carbonation and hydration reaction occurs.

3.4.7 Water Absorption test

This test was conducted based on British Institution Standard (BSI1881: Part 122: 1983). The mould
used to prepare is a cylinder with 50 mm of diameter and 100 mm in height. The cement paste
formulation used was same as in Table 3.1. After preparing the 28 days curing sample, the samples
then dried for 72 ±2 hours at the temperature of 105 ±5℃. After 72 hours of oven heating, the
samples were taken out, cooled it for 24 ±0.5 hours in the dry tight vessel. An empty tin used as a
tight vessel. After 24 hours, the samples were weight by using measuring balance. After initial mass

20
weighted, the samples were soaked in water for 30 ±5 minutes. The samples were weight to obtain
the final weight. Below is the formula used to calculate water absorption of the mortar:

%Absorbent of water= (W F-W I)/WiX100

21
 CHAPTER 4: RESULT AND DISCUSSION

4.1 Analysis for Garnet R mortar

To test the recycled Garnet (Garnet R) mortar, 7 analyses were conducted during the research. The
selection Garnet R was based on ASTM C 311 for natural pozzolan. As Garnet R were used as
replacement to the cement, it is important to determine the compatibility of Garnet R inclusion in
mortar.

4.2 Compressive strength of mortar

According to ASTM C 618-05, recycled Garnet can be used as pozzolan when 28 days strength
activity index of mortar meet the specification compliance.

Table 4.1 Comparability of Strength Activity Index (SAI) of ASTM and analysis result

Strength Activity Index (ASTM C

Compressive 618-05) Strength Activity
Samples strength of 28 Index of Garnet
Class
days, N/mm2 R mortar
N F C

0% 14 -

10% 15 111
75B 75B 75B
20% 11 79

30% 14 100

22
 Average strength of concrete
25

Average stregnth, KN/mm3

20

15

28 days
10
73 days
5

0
0% 10% 20% 30%
Garnet R sample

Figure 4.1 Compressive strength of Garnet R mortars for 28 days and 73 days (error bar represents
Standard Deviation)

The mortar samples were tested using compressive strength machine. The result obtained is
presented in Figure 4.1, shows that the compressive 10% and 30% of Garnet R mortar sample are
higher than control samples (0% Garnet R) while 20% of Garnet R sample is lower than the control
sample. The average value compressive strength for 0%, 10%, 20% and 30% Garnet R is 14.32
N/mm2, 0.01479 N/mm2, 13.43 N/mm2 and 15.97 N/mm2. The result of 20% Garnet R mortar for 28
days may due to the technical error during preparing the sample as shown in Figure 4.1. The mortar
should be uniformly tamped by tamping rod for 25 times, but the tamping was done for 27 times for
mortar of 20% Garnet R. In addition, the excess mortar paste (20% Garnet R) was not properly
removed by tamping rod, resulting in the uneven surface of mortar after 28 days curing as shown in
Figure 4.2.

Figure 4.2 Slanting surface of the mortar before compressive strength test
23
 Siddique et al., (2011) test the compressive strength of concrete with a mixture of cement,
aggregates, silica fumes (SF) and sand. They included 6%, 10% and 15% of SF and obtain
increasing value with 65.0 N/mm2, 67.5 N/mm2, 70.0 N/mm2 of compressive strength which higher
than 58.0 N/mm2 control sample (0% of SF). In other research by Siddique et al., (2009) on mortar
with mixture of cement and metakaolin, they included 5%, 10% and 15% of metakaolin where
compressive strength increases proportionally to the percentage of metakaolin inclusion which is
91.5 N/mm2, 104.0 N/mm2 and 103.5 N/mm2 accordingly to increase in metakaolin inclusion.
Another study by Kanning et al., (2014) on banana leaves ashes (BNA) mortar found that the
compressive strength increase as the BNA inclusion increase. With 5% of BNA inclusion, the
compressive strength value is 33.0 N/mm2, and maintain the value for 7.5% and 10% inclusion
which is 36.0 N/mm2. As a comparison for 10% of pozzolan mortar, Garnet R contributes higher
compressive strength than silica fume and banana leave ashes, but lower than metakaolin.
As the curing age increase, the compressive strength of Garnet R decrease significantly. This
statement is proved by (Hossain et al., 2016) where they observe the loss of compressive strength
of black rice husk ash (BRHA) mortar with the increasing curing age. The change was observed
from day 1 to day 180 which show significant compressive strength loss. Contrarily with Kanning et
al., (2014) where they observed BLA mortar at 28 days, 56 days and 91 days, found that
compressive strength increasing steadily slow as the curing age increase.

4.3 Density

The best density observed was at sample 30% of Garnet R mortar which is 1974.4307 Kg/m3,
compared to 1934 .8821 Kg/m3 of 10% and 1958.1063 Kg/m3 of 20% of Garnet R mortar.

Average measured density

2500

2000
Density, Kg/m3

1500

1000

500

0
Control 10% 20% 30%
Garnet R samples

Figure 4.3 Measured density of 28 days curing mortars (error bar represents Standard Deviation)
24
High density indicates a higher strength of mortar. Holm et al,. (2007) tested that high quality
concretes can maintain low density by limitedly absorbing water. They added that the concrete will
lower in density due to moisture loss where it corresponds to the ambient conditions and surface
area/volume ratio of the concrete.
Besides, water-cement ratio, materials ratio, supplementary cementitious materials, curing,
and type of cement are another parameter that affecting the density and compressive strength of
concrete cement paste (Carolina, 2016). In addition, studied done Amran et al., (2015) on foam-
concrete proves that at high water content, the cement will become slurry and thin which make it
segregate and increase the final density of concrete.
Carolina (2016) adding that as the curing age of concrete increases, the strength and density
also increase and reduces the absorption capacity. Raheem et al., (2013) explained that with proper
curing method, the significance value of density and compressive strength of concrete will be
achieved. Besides, the tendency of compressive strength of concrete will increase as the density of
the concrete increase. Despite control samples (0% Garnet R) has the highest density compared to
other samples, it is due to improper method done during the preparation of mortar samples which
resulting in the different height of each (10%, 20% and 30%) samples.
The density at 30% of Garnet R is very contrast to the lowest compressive strength obtain in
Figure 4.1. It may due to slanting surface of the samples during the compressive strength test which
disturb the reading.

4.4 Carbonation

10 wt.% of phenolphthalein composed by 95% of ethanol and 10 % of water was prepared to test
the carbonation of mortar. The prepared phenolphthalein then is sprayed onto the mortars. The
change of mortar colour was observed in Table 4.2.

Table 4.2 Phenolphthalein Test on mortar

Samples Mortar Description

Carbonation area (arrow) within

A (0% Garnet R) mortar as well as on the outer
surface

25
 Table 4.2 Phenolphthalein Test on mortar

Carbonation area detected

B (0% Garnet R)
(arrow) below the outer of mortar

There are patches of

carbonation area (arrow) inner
C (0% Garnet R)
surface of mortar as well as
outer surface

There are carbonated area

A (10% Garnet R) (arrow) inner surface of mortar
as well as outer surface

No carbonated area at inner

B (10% Garnet R) surface of mortar except outer
surface

Carbonation only occurred on

C (10% Garnet R)
the outer surface

Carbonation only occurred on

A (20% Garnet R)
the outer surface

Carbonation only occurred on

B (20% Garnet R)
the outer surface

26
 Table 4.2 Phenolphthalein Test on mortar

Carbonation only occurred on

C (20% Garnet R)
the outer surface

There are carbonated area

A (30% Garnet R) (arrow) inner surface of mortar
as well as outer surface

Carbonation only occurred on

B (30% Garnet R)
the outer surface

Carbonation only occurred on

C (30% Garnet R)
the outer surface

Only mortar samples with 20% of Garnet R were carbonated at the outer surface, while
carbonation occurs within the mortars of samples A (10% and 30% of Garnet R) and carbonation
occur both inner and outer surface of mortar at control samples (0%).
Carbonation is a common type of attack in cement paste and mortars. The process begins
when CO2 enter the cement mortar, dissolving in the pore solution to produce HCO3- and CO32- ions,
which react with Ca2+ from calcium hydroxide (CH). In addition, calcium silicate hydrate (C–S–H)
and the hydrated calcium aluminates and Ferro aluminates will precipitate and forms various
calcium carbonate (CaCO3), silica gel and hydrated aluminium and iron oxides (Borges et al., 2010).
Torgal et al., (2012) stated that at the uncarbonated area, the specimen will change in colour
to purple-red colour where it is high alkalinity, while the carbonated area will no colouration occur
as the alkalinity reduced. The purple colour surrounds the surface of mortar indicate the area which
carbonation occurs. (Pacheco et al., 2012).The carbonation occurred almost at the outer surface of
Garnet R mortar samples.

27
 This phenomenon occurs might be from several factors such as water binder ratio, porosity,
and permeability of the concrete (Hossain et al., 2016). In addition, Silva et al., (2015) proposed that
the rate of carbonation depends on the permeability, moisture content and relative humidity of the
concrete. By using Garnet R to act as siliceous cementitious material (SCM) in mortar, the results
show that almost 0% rate of carbonation based on Table 4.2.
Peter et al., (2008) studied that the carbon dioxide is in an aqueous state will react with
calcium hydroxide, Ca(OH)2 during carbonation reaction to produce calcium trisilicate, CaSiO3. The
carbonation reaction also produces C-S-H as a product. The formation of CaCO3 will change the
porosity of the concrete as mentioned by Peter et al., (2008).

4.5 pH test

From Figure 4.4, the highest average pH of mortar is at 10% of Garnet R. Mortar with 10% Garnet
R has the highest pH with the value of 13.16 compared with 0%, pH of 13.02, followed by 20%, pH
of 12.99 and 30%, pH of 12.89. Mortar with higher pH usually has a lower possibility to be attacked
by corrosion. Optimum pH value which is 9 enhanced the durability of mortar as the cement will
efficiently hold the mixture or component within the concrete.

pH of Mortar
13.3

13.2

13.1
Average pH

13.0

12.9

12.8

12.7
Control 10% 20% 30%
Garnet R samples

Figure 4.4 pH of mortar (28 days curing) (error bar represents Standard Deviation)

The common pH value of mortar is lower than 9. However, the pH value obtain is high. The
result from Table 4.2 and Figure 4.4 show that high pH value indicate that the carbonation will less
likely occur in the mortar. Hence, chloride attack can be prevented and make the Garnet R mortar

28
to last longer than normal mortar. Rahman (2014) stated that concrete with low quality usually has
pH lower than 9. This statement is proved from the actual result, which the higher the pH, the higher
the mechanical strength, but the actual properties of mortar should have pH lower than 9. Refer to
Figure 4.1, the best compressive strength obtain is at 10% of Garnet R mortar which proves that the
higher the pH, the higher the compressive strength of mortar.

4.6 Moisture content test

To determine the moisture content in the mortar, the oven dying method was applied. Initially, the
samples were weighed before dried for 3 days. Then, final weight was determined. The wet basis
formula is used to determine the moisture content of mortar.

(Weight Initial − Weight Final)

Moisture content = x 100
(Wt. % after − Wt container)

Average Garnet R concrete moisture content

30

25
Average Moisture, g

20

15

10

0
10% 20% 30%
Garnet R samples

Figure 4.5 Moisture content of mortar samples of 28 days curing (error bar represents Standard
Deviation)

Moisture content is one of the factors that influences mortar strength. From the data in Figure
4.5, samples contain 10% of Garnet R has most suitable moisture content. For 0% Garnet R
samples, the data need to be neglected as the value is assumed not valid. Overall, the mortar with
20% Garnet R has the highest moisture content followed by 30% and 10% of Garnet R mortar. This
show that mortar inclusion with 10% of Garnet R has the least moisture content within which can

29
lowering the compressive strength and durability of the mortar. It is due to the compressive strength
test result which produces average 15.9965 N/mm2.
Costigan et al., (2014) stated that mortar with excessive water content has low mechanical
strength and the risk of cracking by shrinkage will be higher. High moisture content will make the
mortar weak as referred to the sample of 20% Garnet R. It may due to higher porosity in the mortar
specimen. Concrete with high porosity will allow more moisture to partly flow in it in two states; liquid
and vapour (Jafarifar et al., 2014). Shoukry et al., (2011) support that water vapour escape the
specimen slowly, but expand quickly and creating vapor pressure. The concrete strength can’t
withstand the increasing amount of vapor pressure over time which causes crack in the internal area
of the concrete sample. The moisture used the crack to escapes from the specimen, putting more
pressure on the outer surface of concrete and eventually will collapse.
As the water moves out from concrete through porosity, the concrete specimen will
shrinkage. Jafarifar et al., (2014) stated the factor that affected the shrinkage are initial curing
condition, relative humidity, condition, volume to surface ratio, concrete composition, air content and
percentage of fine aggregates.

4.7 Water Absorption

The water absorption test is done according to British Standard Institution (BSI1881: Part 122:
1983). The 28 days curing of cylindrical mortar were weighted for initial mass before soaked in the
water at ± 2.5cm above the surface of mortar. After 30 minutes, each mortar was dried with tissue
as replacement of cloth before final weight.

Average water absorption

24

22
Water Absorption, g

20

18

16

14

12

10
0% 10% 20% 30%
Sample of Garnet R Mortar

Figure 4.6 Water absorption of Garnet R mortar (error bar represents Standard Deviation)
30
 The water absorption obtain show that the sample of 20% Garnet R has the highest value
which is 22.51% water absorption compared to other samples. It can be observed that 10% of
Garnet R mortar have 19.54% of water absorptivity is lower than 0% Garnet R mortar (21.5% of
water absorptivity) and 20% Garnet R mortar (13.44% of water absorptivity), while higher than 30%
Garnet R water absorption. A research by Gingos et al., (2011), he found that the pulverized fly ash
(PFA) has higher water absorption at 10% mixture, following declination in 20% and increase slightly
at 30% admixture. Similarly with Siddique et al., (2009), they found that water absorption of
metakaolin mortar increase from 8.78% at 10% metakaolin to 9.71% at 15% metakaolin and
decrease slightly to 9.70% at 20% of metakaolin inclusion. Contrary, Dhinakaran and Chandana
(2016) test the water absorption on bamboo leaf ash (BFA) mortar and found that the water
absorption increases as the percentage of BFA increase from 10%, 20% and 30%.
The higher the percentage of Garnet R mix in the mortar, the lower the water absorption of
mortar. This may due to the siliceous material in Garnet R has already filled up space within the
mortar.

4.8 Thermogravimetric Analysis

TGA was done after carbonation test of mortars. Figure 4.7, 4.8 and 4.9 represent the mass loss by
percentage of Garnet R mortars. This analysis performs under the heating rate of at 10℃/min from
30 to 1100℃.

Figure 4.7 TGA graph for 10% Garnet R sample

31
 Figure 4.8 TGA graph for 20% Garnet R sample

Figure 4.9 TGA graph for 30% Garnet R sample

Mass loss up to 200℃ for 10%, 20% and 30% Garnet R mortar indicate that dehydration occurs as
water loss from the mortar. It can be observed from the drop peak that at 10% of Garnet R mortar

32
has highest mass loss at 9.76% compare to 20% and 30% of Garnet R samples which at 8.10%
and 9.51%.
Portlandite decomposition occurs at the temperature between 420℃ to 490℃. The highest
mass loss obtained is 5.36% at 10% of Garnet R mortar, which higher than 5.00% and 5.12% mass
loss at 20% and 30% Garnet R mortar. At high temperature, dehydration occurs faster than the
lower temperature which means heating rate act as factor. The different heating rate will result in
the different dehydration reaction.
Based on TGA graphs obtained, at the temperature between 600 to 790℃ where the sharp
drop is observed, the carbonation occurs. At 10% of Garnet R sample, the highest rate of
carbonation obtained which is 12.97 % of mass loss compared to 20% and 30% of Garnet R sample
which 11.38 % and 8.01 % mass loss. This is due to the decomposition of CaCO3 into CaO and
CO2 gas. It also indicates that the higher the weight loss, the higher the carbonation reaction in the
mortar. Even though not all Garnet R specimen has carbonation, this proved that carbonation still
occurs in mortar with the inclusion of Garnet R.
TGA proved that Garnet R can be used as pozzolan to replace cement where the mass loss
for hydration, carbonation and portlandite decomposition was observed. However, there are peak
at 850-900℃ at Figure 4.7 and Figure 4.8 which can’t be identified by TGA.

33
 CHAPTER 5: CONCLUSION AND RECOMMENDATION

5.1 Conclusion

This study presents a comprehensive review on compatibility of Garnet R as pozzolan material in

mortar. As general, it can be concluded as follow:
The methodology of preparing cement paste and mortar give significance effect on the
analysis conducted. The durability of the mortar mostly depends on compressive strength, as well
as pH and moisture content. Carbonation, density and water absorption were proved fail to influence
the compressive strength. These parameters were influence verily to compressive strength of
mortar. Moisture content control, 0% Garnet inclusion data were omitted as the error bar were
extremely out of range. TGA graphs were interpret where the carbonation, hydration and
decomposition reaction occur within mortar explained.
From the analysis conducted, it can be deduced that Garnet R can be used to partly replace
cement in mortar as it provides significant data and obey the requirement needed as pozzolan by
ASTM.

5.2 Recommendation

The performance of Garnet R can be enhanced by preparing better condition of mould; precise
height and the bottom surface covered by even plate. By increasing the number of duplicate of each
percentage replacement of Garnet R from 3 to 5, better observation can be done. If there is error
occurs during mortar preparation; slanting surface, it can be solved by comparing only 3 duplicate
of each percentage inclusion.
Another analysis that can be perform is Fourier Transform Infrared Spectroscopy (FTIR)
where it can determine unidentified peak at TGA graph as it determine the composition of solids,
liquids and gases occurred. Besides, chemical analysis also can be conducted to use as quality
control; to detect any faulty of brick.

34
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