STUDY ON THE BEHAVIOUR OF HIGH STRENGTH PALM OIL FUEL

ASH (POFA) CONCRETE

OMAR ELMUKHTAR AHMED ELDAGAL











UNIVERSITI TEKNOLOGI MALAYSIA






iv





STUDY ON THE BEHAVIOUR OF HIGH STRENGTH PALM OIL FUEL
ASH (POFA) CONCRETE





OMAR ELMUKHTAR AHMED ELDAGAL




A project report submitted in partial fulfillment of the
requirements for the award of the degree of
Master of engineering (Civil-Structure)




Faculty of Civil Engineering
Universiti Teknologi Malaysia






NOVEMBER 2008




vi














To my beloved mother



































vii





ACKNOWLEDGEMENT




First and foremost, praise belongs to Allah, the Most Gracious and Most
Merciful Who has created the mankind with knowledge, wisdom and power. Being
the best creation of Allah, one still has to depend on others for many aspects directly
or in directly.

The author would like to take this opportunity to express profound gratitude
to his research supervisors; Associate Prof. Dr. Mohamed Abdelkader El-Gelany
Ismail and Professor Dr. Mohd Warid Hussin for the noble guidance and valuable
advice throughout the period of study. Their patience, time, and understanding are
highly appreciated. The author is also grateful to Dr. Zaiton Abdul Majid for her
consultation in the chemical and thermogravemetric analysis in this study.

The author is thankful to the Yayasan Pembangunan Johor in Ladang Alaf for
the supplying of the palm oil fuel ash. A word of Gratitude is extended to the
technical staff of the several laboratories of the university.

Last but not the least; the author remembers his parents and relatives for their
countless blessing which have always been source of inspiration in achieving success
to this level.









viii



ABSTRACT

Many researchers have studied the use of agro-waste ashes as constituents in
concrete. These agro-waste ashes contained an amount of silica which could be used
as a pozzolanic material. Palm Oil Fuel Ash (POFA) is a by-product produced in
palm oil mills. This ash has pozzolanic properties that not only enables the
replacement of cement but also plays an important role in making strong and durable
concrete. Collected POFA was dried and then sieved through a 300 m sieve. Ashes
passing through 300 m sieve were ground in a modified Los Angeles abrasion test
machine. The fineness of the POFA was checked by sieving through 45m sieve at
every half an hour grinding. For this research, total of five mixes were made of OPC
as a control mix, OPC replaced with 20% and 30 % of POFA 10 m and OPC
replaced with 20 and 30 % of POFA 45 m respectively. For compressive strength,
six cubes of 100 mm tested at 7, 28, and 90 days. For flexural strength, three prisms
of 100 x 100 x 500 mm were tested at 28 days. Five cylinders of 100 x 200 mm were
tested for indirect tensile strength at 28 days for each mix. The slump test and
compacting factor test were employed in measuring the fresh concrete. POFA
concrete exhibit lower value of slump compared to slump of OPC concrete. Among
POFA results, the finer the POFA, the lower the slump and hence lower degree of
compaction. Although strength of POFA concrete did not exceed that of OPC, 58
MPa was achieved when using 20 % of POFA 10 m. The flexural strength of POFA
concrete is slightly lower than that of OPC. The higher was the replacement of OPC;
the lower the flexural strength. Like that of flexural strength, indirect tensile strength
of concrete containing POFA developed in a similar way. TG Analysis lead to the
fact that the amount of Ca(OH)
2
increased with curing age indicating the progress of
cement hydration reaction. And reduction in weight loss attributed to
dehydroxylation of calcium hydroxide, and subsequent increase in compression is
indicative of pozzolanic reaction. From the microstructural analysis (FESEM),
radiating clusters of C-S-H gel have lead to a densification of the structure, and an
increase in strength. Hexagonal platelets of Ca(OH)
2
could be observed in some
samples.
ix
ABSTRAK

Banyak penyelidik telah mengkaji penggunaan abu yang merupakan sisa
industri sebagai bahan dalam pembuatan konkrit. Abu ini mengandungi silica yang
membolehkan ia digunakan sebagai bahan pozolana. Abu kelapa sawit (POFA)
adalah bahan buangan yang dijana oleh kilang memproses kelapa sawit. Abu ini
memiliki sifat-sifat pozolana yang bukan sahaja membolehkan ia berfungsi sebagai
bahan pengganti simen tetapi turut memainkan peranan penting dalam menghasilkan
konkrit yang kuat dan tahan lasak. POFA yang diambil dari kilang telah dikeringkan
dan diayak melepasi ayak 300 m seterusnya dikisar menggunakan mesin pengisar
Los Angeles. Kehalusan POFA kemudian dikenalpasti dangan mengayak abu
tersebut menerusi ayak 45 m pada setiap setengah jam sepanjang pengisaran
dijalankan. Dalam kajian ini, sebanyak lima bancuhan telah dihasilkan iaitu yang
mengandungi simen Portland biasa (OPC) sebagai bancuhan kawalan, OPC yang
diganti dengan 20 % dan 30 % POFA 10 m dan OPC yang diganti dengan 20 % dan
30 % POFA 45 m. Kekuatan mampatan diperolehi dengan menguji enam kiub
bersaiz 100 mm pada 7, 28, dan 90 hari. Kekuatan lenturan pula ditentukan dengan
menguji tiga prisma bersaiz 100 x 100 x 500 mm pada 28 hari. Lima silinder (100 x
200 mm) telah diuji untuk menentukan kekuatan tegangan pada 28 hari bagi setiap
bancuhan. Ujian runtuhan dan ujian faktor pemadatan telah digunakan untuk
menentukan sifat konkrit segar. Konkrit POFA menunjukkan nilai runtuhan yang
rendah berbanding konkrit OPC. Daripada keputusan POFA, semakin halus POFA
maka semakin rendah nilai runtuhan dan nilai pemadatan yang diperolehi. Walaupun
kekuatan POFA tidak mengatasi OPC, kekuatan 58 MPa dapat dicapai apabila
menggunakan 20 % POFA 10 m. Nilai kekuatan lenturan bagi konkrit POFA
adalah sedikit rendah daripada OPC. Semakin tinggi nilai penggatian OPC; semakin
rendah kekuatan lenturan. Kekuatan tegangan konkrit POFA menunjukkan corak
sama seperti yang didapati dalam kekuatan lenturan. Analisis TG yang menunjukkan
kandungan Ca(OH)
2
meningkat dengan umur pengawetan membuktikan
penghidratan simen terus berlaku. Pengurangan dalam kehilangan berat adalah
disebabkan dehydroxylation kalsium hidroksida manakala peningkatan kekuatan
mampatan membuktikan berlakuanya tindak balas pozolana. Berdasarkan analisis
mikrostruktur (FESEM), perkembangan dalam kelompok C-S-H gel telah membawa
kepada pemadatan struktur dan meningkatkan kekuatan.
x





CONTENT


CHAPTER SUBJECT PAGE


CERTIFICATION OF THESIS ii
CERTIFICATION BY SUPERVISOR iii
TITLE PAGE iv
AUTHORS DECLARATION v
DEDICATION vi
ACKNOWLEDGEMENTS vii
ABSTRACT viii
ABSTRAK ix
CONTENTS x
LIST OF TABLES xiii
LIST OF FIGURES xiv
LIST OF ABBREVIATIONS SYMBOLS AND xvi

I INTRODUCTION

1.1 Introduction 1
1.2 Background of Research 2
1.3 Objectives of Research 4
1.4 Scope and Limitation 4
1.5 Importance of Research 4
1.5.1 Advantages of High Strength Concrete 5



xi
II LITERATURE REVIEW

2.1 Cement Replacement Materials 7
2.2 Pozzolanic Materials 8
2.3 Pozzolanic Behavior 9
2.4 Types of Pozzolanic Materials 10
2.5 Origin of Palm Oil Fuel Ash 10
2.6 Pozzolanicity of Palm Oil Fuel Ash 11
2.7 Effect of Fineness of the POFA 11
2.8 Effect of Ash Content 12
2.9 Strength Development 13

III EXPERIMENTAL PROGRAMME AND MATERIAL
PROPERTIES

3.1 Introduction 15
3.2 Selection of Materials 15
3.2.1 Cement 16
3.2.2 Palm Oil Fuel Ash (POFA) 17
3.2.2.1 Preparation of the POFA 18
3.2.2.2 Fineness of the POFA 19
3.2.3 Aggregate 21
3.2.3.1 The Coarse Aggregate 22
3.2.3.2 The fine Aggregate 22
3.2.4 Water 23
3.3 Mix Proportions 24
3.3.1 Number of Specimens for Each Mix 24
3.4 Superplasticizer 26
3.5 Measurement of Workability 27
3.5.1 Slump Test 27
3.5.2 Compacting Factor Test 29
3.6 Curing 30
3.7 Tests on Hardened Concrete 31
3.7.1 Compressive Strength 31
xii
3.7.2 Flexural Strength Test 32
3.7.3 Splitting Tensile Test 33
3.8 Thermogravimetric (TG) Analysis 34
3.9 Microstructural Analysis 35

IV RESULTS AND DISCUSSION

4.1 Introduction 36
4.2 Slump Test Result 36
4.3 Compacting Factor Results 38
4.4 Compressive Strength 38
4.5 Flexural Strength Results 41
4.6 Splitting Tensile Test Results 42
4.7 Chemical Analysis of POFA and OPC 43
4.8 Thermogravimetric Analysis 44
4.9 Microstructural Analysis (FESEM) 46
4.10 Summary 52

V CONCLUSIONS AND RECOMMENDATIONS

5.1 Introduction 53
5.2 Behavior of POFA Concrete in the Fresh State 53
5.3 Behavior of POFA Concrete in the Hardened State 54
5.4 Thermogravimetric analysis (TGA) 54
5.5 Microstructural Analysis (FESEM) 54
5.6 Recommendations for Future Investigation 55

REFERENCES 56






xiii





LIST OF TABLES PAGE




Table 3.1: Chemical composition of OPC and Palm Oil Fuel Ash 14
Table 3.2: Grinding time vs. the mean diameter of POFA 18
Table 3.3: Quantities of the constituents per cubic meter 22
Table 3.4: The tests, number of specimens and ages for each test 23
Table 3.5: Correlation of compaction factor test results to slump test results 28

Table 4.1: Compressive strength results 36
Table 4.2: Chemical composition of OPC and POFA 44
Table 4.3: The percent weight loss for P
1
, P
2
, P
3
, and P
4
45
Table 4.4: Thermogravimetry data for Po, P1, P2, P3 and P4 at 90-days
curing age 45














xiv





LIST OF FIGURES PAGE




Figure 1.1: Palm oil shell ad fiber

Figure 2.1: Effect of fineness of ash on compressive strength of concrete 10
Figure 2.2: Effect of ash content on compressive strength of concrete at
28 days 11
Figure 2.3: Strength development of OPC and POFA concretes 12

Figure 3.1: The palm oil mill 15
Figure 3.2: Ash where trapped at the flue of tower 16
Figure3.3: Flow-chart for the manufacture of POFA 17
Figure 3.4: Effect of grinding time on fineness of POFA 18
Figure 3.5: CILAS 1180 Liquid instrument 19
Figure 3.6: The coarse aggregate 20
Figure 3.7: The fine Aggregate 21
Figure 3.8: Slump test apparatus 26
Figure 3.9: Compacting factor apparatus 27
Figure 3.10: Curing of samples in water 28
Figure 3.11: Compression test machine 29
Figure 3.12: Flexural test machine 30
Figure 3.13: Concrete cylinder after testing for tension 31

Figure 4.1: Slump test results 34
Figure 4.2: Compacting factor results 35
Figure 4.3: Relationship between compressive strength results 37
Figure 4.4: Flexural strength results 38
Figure 4.5: Splitting tensile strength results 39
xv
Figure 4.6: FESEM of P
4
at 3 days using 1000X magnification showing
porous morphology. 43
Figure 4.7: Granules of POFA when using 1000 X magnification of
P
3
at 3 days 44
Figure 4.8: FESEM of P
3
at 7 days using 2000X magnification 45
Figure 4.9: FESEM, P
2
at 7 days, hexagonal platelets of Ca(OH)
2
45
Figure 4.10: Microstructure of P
3
at 3 days at 500, 1000, and 2000 X
magnification 46
Figure 4.11: Microstructure of P
3
at 7 days at 500, 1000, and 2000 X
magnification 47


































xvi





LIST OF ABBREVIATIONS AND SYMBOLS




Abbreviations:

ACI = American Concrete Institute
ASTM = American Society for Testing and Materials
BS = British Standards
CSF = Condensed Silica Fume
DOE = Department of Environment
FESEM = Field Emission Scanning Electron Microscopy
GGBS = Ground Granulated Blast furnace Slag
LOI = Loss on Ignition
OPC = Ordinary Portland Cement
PFA = Pulverised Fuel Ash
TGA = Thermogravimetric Analysis




Symbols:

Al
2
O
3
= Aluminium Oxide
C
2
S = Dicalcium Silicate
C
3
A = Tricalcium Aluminate
C
3
S = Tricalcium Silicate
CaCO
3
= Calcium Carbonate
CaO = Calcium Oxide
xvii
Ca(OH)
2
= Calcium Hydroxide
CaO = Calcium Oxide
CO
2
= Carbon Dioxide
CH = Calcium Hydrate
C-S-H = Calcium Silicate Hydrate
Fe
2
O
3
=

Ferric Oxide
SiO
2
= Silicon Oxide
K
2
O = Potassium Oxide
MgO = Magnesium Oxide
MnO
3
=

Magnesium Trioxide
Na
2
O = Sodium Oxide
SMF = Sulfonated Melamine Formaldehyde
SNF = Sulfonated Naphthalene Formaldehyde

1




CHAPTER I




INTRODUCTION



1.1 Introduction


Concrete is one of the oldest manufactured construction material used in
construction of various structures around the world. However, continuous research in
the area of concrete material has resulted in production of many types of concrete
known in various names each having a unique characteristic to fulfill the current
construction industry demand. One of the concrete that become famous nowadays is
high strength concrete due to its strength and durability (Abdullah and Hussin, 2006).



Although high strength concrete is often considered a relatively new material,
its development has been gradual over many years. As the development has
continued, the definition of high-strength concrete has changed. In the 1950s,
concrete with a compressive strength of 34 MPa was considered high strength. For
many years, concrete with compressive strength in excess of 41 MPa was available at
only a few locations. However, in recent years, the applications of high-strength
concrete have increased, and high strength concrete has now been used in many parts
of the world (ACI, 1992).

2

In order to achieve high strength concretes, several methods can be applied.
In general, high strength concrete contains strong aggregates, a higher Portland
cement content and low water cement or water cementitious ratio. The addition of
water reducing admixtures, superplasicizers, blast furnace slag, or silica fume is
common today (Nawy, 1996).


Savings in overall cost of concrete structural systems are achieved by the use
of higher strength concretes. Components of structure become smaller, thereby
reducing the weight of the system with the resulting reduction in size and then cost of
all components. The use of cement replacement materials in producing high strength
concrete also encouraged sustainable development as it reduces the cement usage. As
some cement replacement materials are obtained from agricultural wastes, it also
helps recycling the by-products (Nawy, 1996).




1.2 Background of Research


Palm oil has been gaining increasing importance as cash crop in several
tropical countries among which Malaysia is the largest producer of palm oil products.
To date there are more than two hundred mills operating in this country (Hussin and
Awal, 1997).


The palm oil industry is one of the major agro-industries in Malaysia. The
commercial palm oil production is mainly located in Peninsular Malaysia and date
back to the 1960s. During the period between 1990 and 2002, palm oil production
was nearly doubled from 6,094,622 to 11,880,000 ton per year, making Malaysia the
biggest palm oil producer worldwide (Vijayaraghavan, 2007).


3

It has been reported that the production of palm oil per month is over 435000
tons, 10 % of which is waste by-product of milling process in the form of palm oil
fibre and palm oil shell as shown in Figure (1.1). These by-products are commonly
known as palm oil fuel ash (POFA), are disposed without any commercial return. It
has been identified that this ash has pozzolanic properties that not only enables the
replacement of cement but also plays an active role in making strong and durable
concrete (Hussin and Awal, 1997).




b) Palm oil fibre















a) Palm oil shell









































Figure 1.1: Palm oil shell and fibre
4

1.3 Objectives of Research


The main objective of this present research is to study the behavior of high
strength concrete by using palm oil fuel ash (POFA) in different fineness as partial
replacement of ordinary Portland cement. In addition to this, study the effect of
POFA on the workability of concrete.




1.4 Scope and Limitation


All test specimens are made up of concrete where Ordinary Portland cement
is replaced with 20 % and 30 % of POFA 10 m, and 20 % and 30 % of POFA 45
m. Compressive, flexural, and tensile strengths are the major tests considered for
determining the strength of concrete. Slump and compacting factor, on the other
hand, are the tests to measure the workability of the concrete.




1.5 Importance of Research


The accelerated developments in concrete research over the past 20 years
have opened new and more proficient utilization of components available in nature,
including industrial waste. The thrust in this accelerated activity has been made or
justified because of the economical gains in producing stronger structures that are
smaller in component dimensions while larger in resulting space availability. Cost
analysis of the use of high strength concrete as compared to normal strength concrete
justifies its viability and utility (Nawy, 1996).

5


In recent years, studies have been carried out by various researchers in using
wastes generated from the agricultural and industrial activities as concrete making
materials (Tay and Show, 1994).


Many researchers have studied the use of agro-waste ashes as constituents in
concrete. Their results have revealed that these agro-waste ashes contain high
amount of silica in amorphous form and could be used as a pozzolanic material
(Tangchirapat and Saeting, 2007). Utilization of palm oil fuel ash (POFA) is minimal
and unmanageable, while its quantity increases annually and most of the POFA are
disposed of as waste in landfills causing environmental and other problems
(Tangchirapat and Saeting, 2007). To solve the energy problems, solid wastes from
palm oil residue are used as fuel to produce steam for electricity generation. After
burning, an ash by-product is produced. As a solution to the disposal problem of the
ash derived from palm oil, research studies have been carried out to examine the
feasibility of using the ash as cement replacement materials (Tay and Show, 1994).




1.5.1 Advantages of High Strength Concrete


The advantages of using high strength concrete often balance the increase in
material cost. The following are some advantages that can be accomplished (Nawy,
1996):

1. Reduction in member size, resulting in an increase in rentable space
and reduction in the volume of produced concrete with the
accompanying saving in construction time.
2. Superior long-term service performance under static, dynamic, and
fatigue loading.
3. Low creep and shrinkage.
6

4. Greater stiffness as a result of a higher modulus of elasticity.
5. Higher resistances to freezing and thawing, chemical attack, and
significantly improve long-term durability and crack propagation.































7






CHAPTER II




LITERATURE REVIEW




2.1 Cement Replacement Materials


Cement replacement materials (Illston and Domone, 2001) are those which
used as a substitute for some of the Portland cement in a concrete; partial cement
replacement materials are therefore a more accurate but less convenient name. There
are also a number of other names for this group of materials, including
supplementary cementitious materials, cement extenders, mineral admixtures,
mineral additives, latent hydraulic materials or, simply, cementitious materials.


Several types of materials are common in use, some of which are by-products
from other industrial processes, and hence their use may have economic advantages.
However, the main reason for their use is that they can give a variety of useful
enhancements of or modifications to the concrete properties. All the materials have
two common features; their particle size range is similar to or smaller than that of
Portland cement, also they become involved in the hydration reactions. They can be
supplied either as individual materials and added to the concrete at mixing, or as pre-
blended mixtures with the Portland cement. The former case allows choice of the rate
of addition, but means that an extra material must be handled at the batching plant; a
8

pre-blended mixture overcomes the handling problem but the addition rate is fixed.
Pre-blended mixtures have the alternative names of extended cements, Portland
composite cements or blended Portland cements. Generally, only one material is used
in conjunction with the Portland cement, but there are an increasing number of
examples of the combined use of two or even three materials for particular
applications.


The incorporation of Cement Replacement Materials leads to a rethink about
the definition and use of the water/cement ratio, which is an important controlling
factor for many properties of hardened cement paste and concrete. It is generally
accepted that this should remain as the ratio of the amount of mix water to that of the
Portland cement, and the term water/binder ratio should be used for the ratio of the
amount of mix water to the sum of the amounts of all of the cementitious materials,
i.e. the Portland cement plus the Cement Replacement Materials.




2.2 Pozzolanic Materials


A pozzolana (Neville, 2005) is a siliceous or siliceous and aluminous
material which in itself possesses little or no cementitious value but will, in finely
divided form and in the presence of moisture, chemically react with calcium
hydroxide at ordinary temperatures to form compounds possessing cementitious
properties.







9

2.3 Pozzolanic Behaviour


A common feature of nearly all Cement Replacement Materials is that they
exhibit pozzolanic behavior to a greater or lesser extent, and so we will define this
before discussing the individual materials (Illston and Domone, 2001). A pozzolanic
material is one which contains active silica (SiO
2
) and is not cementitious by itself,
but will, in a finely divided form, and in the presence of moisture, chemically reacts
with calcium hydroxide at ordinary temperatures to form cementitious compounds.
The key to the pozzolanic behavior is the structure of the silica; this must be in a
glassy or amorphous form with a disordered structure, which is formed in rapid
cooling from a molten state. A uniform crystalline structure which is formed in
slower cooling, such as is found in silica sand, is not chemically active. Naturally
occurring pozzolanic materials were used in early concretes, as mentioned in the
Introduction to this part of the book, but when a pozzolanic material is used in
conjunction with a Portland cement, the calcium hydroxide that takes part in the
pozzolanic reaction is that produced from the cement hydration. Further quantities of
calcium silicate hydrate are produced:


2S + 3CH C
3
S
2
H
3
(2.1)


The reaction is clearly secondary to the hydration of the Portland cement,
which has lead to the name latent hydraulic material in the list of alternatives
above. The products of the pozzolanic reaction cannot be distinguished from those of
the primary cement hydration, and therefore make their own contribution to the
strength and other properties of the hardened cement paste and concrete.






10

2.4 Types of Pozzolanic Materials


There are many types of the pozzolanic material (Illston and Domone, 2001).
The main cement replacement materials in use world-wide are:
1. Pulverized fuel ash (PFA); called fly ash in several countries; the ash
from pulverized coal used to fire power stations, collected from the
exhaust gases before discharge to the atmosphere; only selected ashes
have a suitable composition and particle size range for use in concrete;
2. Ground granulated blast furnace slag (GGBS); slag from the scum formed
in iron smelting in a blast furnace, which is rapidly cooled in water and
ground to a similar fineness to Portland cement;
3. Condensed silica fume (CSF); often called microsilica, extremely fine
particles of silica condensed from the waste gases given off in the
production of silicon metal;
4. Calcined clay or shale; a clay or shale heated, rapidly cooled and ground;
5. Rice husk ash; ash from the controlled burning of rice husks after the rice
grains have been separated;
6. Natural pozzolans; some volcanic ashes and diatomaceous earth.




2.5 Origin of Palm Oil Fuel Ash


Palm oil fuel ash is a by-product produced in palm oil mill. After palm oil is
extracted from the palm oil fruit, both palm oil husk and palm oil shell are burned as
fuel in the boiler of palm oil mill. Generally, after combustion about 5 % palm oil
fuel ash by weight of solid wastes is produced (Abdullah and Hussin, 2006).


The ash produced sometimes varies in tone of colour from whitish grey to
darker shade based on the carbon content in it. In other words, the physical
11

characteristic of POFA is very much influenced by the operating system in palm oil
factory. In practice, POFA produced in Malaysian palm oil mill is dumped as waste
without any profitable return (Abdullah and Hussin, 2006).




2.6 Pozzolanicity of Palm Oil Fuel Ash


The pozzolanicity of any material is closely related to the ability of silica to
react with calcium hydroxide to produce calcium silicate hydrate. For an assessment
of pozzolanic activity with cement, the method of pzzolanic activity index which
determines the totals activity of pozzolana (Neville, 2005). The pozzolanic activity
indices of palm oil fuel ash was obtained by (Abu, 1990) and (Sumadi and Hussin
1993) are 78.6 and 87.6 % respectively. However, for all classes of ash; the
pozzolanic activity is 75 % (ASTM C 618-94 a).




2.7 Effect of Fineness of the POFA


In order to achieve better strength of concrete consisting POFA, Awal and
Hussin (1996) have been suggested that finer POFA is to be used. By increasing the
fineness of POFA would lead to greater strength development than the coarser one.
In Fig 2.1, it can be seen that lower development in strength with coarse ash. And
that was due its lower surface area of the particle that affect the pozzolanic activity
and hence the strength.




12











26.5
35.5





49
0
10
20
30
40
50
60
100% Passing 600
m , Unground
(Coarse)
100% Passing 300
m , Unground
(Medium)
85% Passing 45 m
, Ground (Fine)
2
8
-
D
a
y
s

C
o
m
p
r
e
s
s
i
v
e

S
t
r
e
n
g
t
h

(
M
P
a
)
Ty e of Ash p

Figure 2.1: Effect of fineness of ash on compressive strength of concrete (Awal,
1998)




2.8 Effect of Ash Content


Beside the effect of particle size of POFA, the material replacement level also
confirmed as one of the factors that could influence the strength of this concrete.
Using ground POFA of 45 m, Awal and Hussin (1997) proved that maximum
strength can be obtained at replacement level of 30 % which is about 10 % higher
than control one. It also has been found that this material could be added as partial
cement replacement material up to 40 % without any adverse effect on strength of
concrete. However, further increase in the ash content would reduce the strength of
concrete gradually (Awal and Hussin, 1996). The effect of POFA replacement level
towards the strength is presented in Figure 2.2.





13












0
10
20
30
40
50
60
70
0 20 40 60 80
2
8
-
D
a
y

C
o
m
p
r
e
s
s
i
v
e

S
t
r
e
n
g
t
h

(
M
p
a
)
Ash Content (%)
Figure 2.2: Effect of ash content on compressive strength of concrete at 28
days (Awal, 1998)




2.9 Strength Development


POFA concrete is weaker at early age, but at later ages the compressive
strength is found to be higher than that of OPC concrete (Awal and Hussin, 1997) as
shown in figure 2.3. In general, specimens consisting POFA exhibit lesser strength at
early age but compressive continue to increase as curing age become higher. This is
because pozzolana starts reacting somewhat belatedly with the calcium hydroxide
produced by clinker hydration and therefore it behaves like an inert diluting agent
towards the Portland cement with which it has been mixed (Massaza, 1993).







14











0
10
20
30
40
50
60
70
0 10 20 30 40 50
Fig 2.3: Strength development of OPC and POFA concretes (Awal and Hussin, 1997)























60 70 80 90 100
C
o
m
p
r
e
s
s
i
v
e

S
t
r
e
n
g
t
h

(
M
P
a
)
Curing Period ( days)
OPC
POFA
15







CHAPTER III




EXPERIMENTAL PROGRAMME AND MATERIAL
PROPERTIES




3.1 Introduction


This chapter explains the research that has been carried out. All of the
calculation and equation details are explained in this part. Few lab tests were done to
achieve the objective of this research as discussed in chapter one. Consequently, this
chapter has drawn a clear picture and shows how to achieve the research objective.




3.2 Selection of Materials


High strength concrete has been produced using a wide range of quality
materials based on the result of trial mixes. The production of high strength concrete
that consistently meet the requirements for workability and strength development
16

places more stringent requirements on material selection than for normal strength
concretes. Quality materials are needed and specifications require enforcement.




3.2.1 Cement


Ordinary Portland cement was used in this study. It is highly durable and
produces high compressive strengths in mortars and concretes. Portland cement is
hydraulic cement that hardens by interacting with water and forms a water-resisting
compound when it receives its final set.


Portland cement (Nawy 1996) is made of finely powdered crystalline
minerals composed primarily of calcium and aluminum silicates. The addition of
water to these minerals produces a paste which, when hardened, becomes of
stonelike strength. Portland cement is made to meet the specification requirements of
ASTM C 150 for types I, II, III, IV, and V. Table 3.1 shows the chemical
composition of palm oil fuel ash and OPC.


Table 3.1: Chemical Composition of OPC and Palm Oil Fuel Ash

Chemical Composition POFA OPC
Silica (SiO
2
) 48.99 21.45
Aluminium Oxide (Al
2
O
3
) 3.78 3.62
Ferric Oxide (Fe
2
O
3
) 4.89 3.50
Calcium Oxide (CaO) 11.69 60.98
Magnesium Oxide (MgO) 1.22 0.59
Sodium Oxide (Na
2
O) 0.73 0.25
Potassium Oxide (K
2
O) 4.01 0.51
Magnesium Oxide (MnO
3
) 0.01 0.25
Loss on Ignition (LOI) 10.51 1.37









17

3.2.2 Palm Oil Fuel Ash (POFA)


Palm oil fuel ash is a waste product obtained in the form of ash when burning
palm oil husk or fiber and palm kernel shell as fuel in palm oil mill boilers. POFA
which used in this study was collected from a factory processing palm oil owned by
Yayasan Pembangunan Johor in Ladang Alaf at the area of Bukit Lawang, Johor
Darul Takzim as can be seen in Figure 3.1. The ash was found at the flue of tower
where all the fine ashes that were trapped while escaping from the burning chamber
of the boiler. Figure 3.2 shows the ash trapped at the flue of tower of the mill.
Among the available ashes there, only the one looks grayish were sorted out and
collected.


















Figure 3.1: The palm oil mill




18














Figure 3.2: Ash where trapped at the flue of tower



3.2.2.1 Preparation of the POFA


Firstly, collected POFA was dried in the oven at temperature of 110 C 5
for 24 hours in order to remove moisture from it. Secondly, the dried POFA was
sieved through a 300 m in order to remove any foreign material and bigger size ash
particles. After that, only the fine ashes which pass through 300 m sieve is collected
and ground in a modified Los Angeles abrasion test machine having 10 stainless steel
bars which each of them is 12 mm diameter and 800 mm long in order to acquire
finer particles. Figure 3.3 shows flow-chart for the manufacture of POFA.


19

DRYING IN OVEN
SIEVE THROUGH 300 m SIEVE
GRIND IN MACHINE
POFA
ASH FROM THE MILL

Figure 3.3: Flow-chart for the manufacture of POFA




3.2.2.2 Fineness of the POFA


The fineness of the POFA was checked by sieving through 45 m sieve at
every half an hour grinding of 4 Kg ash. Figure 3.4 shows that, by continuing
grinding, the fineness of the ash was obviously found to be increased. The ASTM C
618-94a stated that the maximum amount of all classes of mineral admixtures that
can be retained when using wet sieving on 45 m is 34 %. In other words, 66 % of
the total ash should pass through that sieve. In this project, the time of grinding was
maintained at 3.5 hours for all the grinding operations for 45 m throughout the
project.





20



0
20
40
60
80
100
120
0 2 4 6 8
P
e
r
c
e
n
t
a
g
e

P
a
s
s
i
n
g

%
GrindingTime(hrs)
10
Figure 3.4: Effect of grinding time on fineness of POFA



For ashes finer than 45 m the fineness was checked by using the particle-
size analyzer called CILAS 1180 Liquid as can be seen in figure 3.5. The CILAS
1180 uses a new patented technology. The table below shows the mean diameter for
the grinding hours beyond 7 hours. The time of grinding maintained at 11 hours to
get 10 m throughout the project.


Table 3.2: Grinding time vs. the mean diameter of POFA

Grinding Time (hrs) Mean Diameter ( m)
7 16.74
9 11.09
11 8.46
13 8.41
15 8.34
17 7.65




21


Figure 3.5: CILAS 1180 Liquid instrument




3.2.3 Aggregate


Aggregates (Nawy, 1996) are those parts of the concrete that constitute the
bulk of the finished product. They comprise about 60 to 80 % of the volume of the
concrete and have to be so graded that the entire mass of concrete acts as a relatively
solid, homogeneous, dense combination, with the smaller sizes acting as an inert
filler of the voids that exist between the larger particles.


For optimum compressive strength with high cement content and low water
cement ratio the maximum size of coarse aggregate should be kept to a minimum.
(Al-Oraimi et al., 2005) observed that the compressive strength increased as the
maximum aggregate size decreased.





22

3.2.3.1 The Coarse Aggregate


The coarse aggregate was air dried to obtain saturated surface dry condition
to ensure that water cement ratio was not affected. Few characteristics of aggregate
that affect the workability and bond between concrete matrix are shape, texture,
gradation and moisture content. In this study crushed aggregates from quarry with
the nominal size 10 mm in accordance to BS 882, 1992 were used. Figure 3.6 shows
the coarse aggregate used.



Figure 3.6: The Coarse Aggregate




3.2.3.2 The Fine Aggregate


Fine aggregate is commonly known as sand should comply with coarse,
medium, or fine grading requirements. The fine aggregate was saturated surface dry
23

condition to ensure the water cement ratio is not affected. In this study, sand was
used and sieve analysis was done prior to using it to determine the fine aggregate
passing 600 m sieve. This was the percentage needed for the mix design
calculation. Figure 3.7 shows the fine aggregate used.















Figure 3.7: The Fine Aggregate




3.2.4 Water


In the production of concrete, water plays very important role. The water
used should not contain any substance that might affect the hydration of cement and
affect the durability of concrete. Generally, supplied tap water will be used
throughout the study in mixing, curing and other purposes.



24

3.3 Mix Proportions


Mixture proportioning of high strength concrete is more significant process
than in normal strength concrete. In order to achieve high strength concrete, a higher
Portland cement content, a low water/cement or water/cementitious ratio,
incorporating pozzolanic admixtures, and an addition of water reducing admixtures
are considered essential. Method of design used in designing the mix is according to
Department of Environment ( DOE) United Kingdom. According to this method, the
mix design used in this research is shown in figure 3.3.


Table 3.3: Quantities of the constituents per cubic metre.

Constituents Weight (Kg / m
3
)
Cement 450
Water 195
Fine aggregate 800
Coarse aggregate 900



3.3.1 Number of Specimens for Each Mix


For this research, total of five mixes were caste of ordinary Portland cement
OPC as a control mix, OPC replaced with 20 % and 30 % of POFA 10 m, and OPC
replaced with 20 % and 30 % of POFA 45 m. For compressive strength, 100 mm
cubes were cast and a minimum of five specimens were tested for each age in a
particular mix. For flexural strength, concrete prisms of 100 x 100 x 500 mm
dimensions were prepared and number of specimens for each age in a particular mix
was three. Cylinder specimens of 100 x 200 mm size were made for testing splitting
25

tensile strength and number of specimens was five. For both compressive and
flexural tests were conducted at the ages of 7, 28 and 90 days. Table 3.4 shows the
ages of the different test conducted in the project, the specimen used and the number
of the specimen for each mix.


All freshly cast specimens were left in the molds for 24 hours before being
demolded and then submerged into water for curing until it is time to be tested. All
methods of sampling, making and testing of specimens will be in accordance with
BS1881: Part 116 and Part 118.


Table 3.4: The tests, number of specimens and ages for each test.


Test

specimen

Number of specimens

P0

P1 P2 P3 P4
compressive
strength
7 days Cube
100x100x100
mm
5 5 5 5 5
28
days
5 5 5 5 5
90
days
5 5 5 5 5
Splitting tensile test at
28 days
Cylinder
100x200 mm
5 5 5 5 5
Flexural at 28 days Prism 500
x100x100
mm
3 3 3 3 3

Where:
Which: P
0
= OPC only, P
1
= OPC + 20 % of 10 m POFA, P
2
= OPC + 30 % of 10
m POFA, P
3
= OPC + 20 % of 45 m POFA, and P
4
= OPC + 30 5 of 45 m POFA.





26

3.4 Superplasticizer


The superplasticizers (Roger and Noel, 2002), are a special category of water-
reducing agents in that they are formulated from materials that allow much greater
water reductions, or alternatively extreme workability of concrete in which they are
incorporated. This is achieved without undesirable side effects such as excessive air
entrainment or set retardation. The materials originally developed as the basis for
superplasticizers in the 1960s were sulfonated naphthalene formaldehyde (SNF) and
sulfonated melamine formaldehyde (SMF) in Japan and Germany respectively,
which have found increasing application world-wide over the intervening years. In
the early 1980s, work began on designing polyacrylate-based polymers for
superplasticizer formulations and after some difficulties with severe retardation, and
in some cases excessive air entrainment, products began to appear in the
marketplace, initially in Germany, and then in Japan and the United States. The
polyacrylate-based products are based on three different types of polymer and are
being heralded as the next generation of superplasticizers.


The interaction of superplasticizers with Portland cement is the most
complicated situation of all because of reactions between the various components of
the cement and the competition, for example between the superplasticizer and
gypsum for reaction with C
3
A. However, in general, the hydration is retarded in a
similar manner to the individual components. The C
3
S phase is not as strongly
retarded as for the individual material because the C
3
A strongly adsorbs a large
proportion of the superplasticizer preferentially. And as a result, the formation of
ettringite is accelerated and the higher the molecular weight of SNF, the greater the
retardation of cement hydration (Roger and Noel, 2002).


In this present study, a high-range water reducing chemical admixture known
as Sulfonated Naphthalene Formaldehyde condensate in the form of dry powder was
integrated during the preparation of concrete mix throughout this research. It was
27

type F high-range water reducing admixture complying with ASTM C494-05a. The
percentage of superplasticizer used in this research is 0.35 % of (cement + POFA).




3.5 Measurement of Workability


There is no acceptable test which will measure directly the workability of
concrete. Numerous attempts have been made, however, to correlate workability with
some easily measurement, but none of fully satisfactory although they may provide a
useful information within a range of Variation in workability (Neville, 2005).


It is important that the specimens of concrete that is tested to be
representative specimens. If it is not, then the results obtained by testing will not
represent the concrete placed. ASTM makes provision for sampling fresh concrete in
C172. It spells out procedures for sampling various production systems and specifies
a sample size of 1 cubic ft except for routine Slump and Compacting factor tests. The
specimen must be tested within 15 minutes and during testing must be protected from
the weather.




3.5.1 Slump Test


ASTM C143 test for slump of Portland cement concrete details the procedure
for performing Slump tests on fresh concrete. A slump cone is filled in three layers
of equal volume so the first layer is about 4 in. (76 mm) high, and the second layer is
6 in. (155 mm) high. Each layer is rodded 25 times with a tamping rod 24 in. (600
mm) long and 0.63 in. (16 mm) diameter, with a hemispherical tip with 16mm
28

diameter. The rodding is uniformly distributed and full depth for the first layer and
just penetrating previous layers for the second and third layers. If the level of
concrete falls below the top of the cone during the last rodding, additional concrete is
required to keep an excess above the top of the mold. Strike off the surface of
concrete by a screeding motion and rolling the rod across the top of the cone. In 5 2
seconds, raise the cone straight up. Set the slump cone next to the concrete, and
measure the difference in height between the slump cone and the original center of
the specimen. With the rod set on the cone, this slump measurement can be read to
the nearest 0.23 in. (6mm). The test from filling of the slump cone to measuring the
slump should take no longer than 2 minutes. If two consecutive tests on a sample
show a falling away of a portion of the sample, the concrete probably lacks the
cohesiveness for the Slump test to be applicable. Figure 3.8 shows the slump test
apparatus.














Figure 3.8: Slump test apparatus






29

3.5.2 Compacting Factor Test


The compaction factor test (Neville, 2005) measures the degree of
compaction resulting from the application of a standard amount of work. The test
was developed in Britain in the late 1940s and has been standardized as British
Standard 1881-103, 1993. The apparatus, which is commercially available, consist of
a rigid frame that supports two conical hoppers vertically aligned above each other
and mounted above a cylinder, as shown in Figure 3.9, the top hopper is slightly
larger than the bottom hopper, while the cylinder is smaller in volume than both
hoppers. To perform the test, the top hopper is filled with concrete but not
compacted. The door on the bottom of the top hopper is opened and the concrete is
allowed to drop into the lower hopper. Once all of the concrete has fallen from the
top hopper, the door on the lower hopper is opened to allow the concrete to fall to the
bottom cylinder. A tamping rod can be used to force especially cohesive concretes
through the hoppers. The excess concrete is carefully struck off the top of the
cylinder and the mass of the concrete in the cylinder is recorded. This mass is
compared to the mass of fully compacted concrete in the same cylinder achieved
with hand rodding or vibration.














Figure 3.9: Compacting Factor Apparatus
30

The compaction factor is defined as the ratio of the mass of the concrete
compacted in the compaction factor apparatus to the mass of the fully compacted
concrete. The standard test apparatus, described above, is appropriate for maximum
aggregate sizes of up to 20 mm. A larger apparatus is available for concretes with
maximum aggregate sizes of up to 40 mm.


The results of the compaction factor test can be correlated to slump. Table 3.5
relates the results of the compaction factor test to slump and the samples degree of
workability.



Table 3.5: Correlation of compaction factor test results to slump test results

Description of
workability
Compacting factor Corresponding slump
(mm)
Very low 0.78 0-25
Low 0.85 25-50
Medium 0.92 50-100
High 0.95 100-175




3.6 Curing


Water curing of high strength concrete is highly recommended due to low
water / cement ratio. For this research, water curing will be done on specimens by
fully submerging in water after demolding until testing need to be done. Figure 3.10
shows the curing of the concrete specimens in the water.



31












Figure 3.10: Curing of samples in water




3.7 Tests on Hardened Concrete


In this present research, the investigation of various aspects of strength
behavior of concrete containing palm oil fuel ash. Except for determination of
flexural and tensile strengths, the investigation of strength was mainly to test for
compression.




3.7.1 Compressive Strength


The compression test was conducted by using compressive test machine at
the material lab of Civil Engineering Faculty of the university as specified in the test
method BS 1881-Part 116,1983. An increasing compressive load was applied to the
specimen until failure occurred to obtain the maximum compressive load. The
32

specimen dimension was taken before the testing. The testing was carried out 7, 28,
and 90 days curing as shown in Table 3.4. Figure 3.11 shows the compression test
machine.













Figure 3.11: Compression test machine




3.7.2 Flexural Strength Test


Flexural strength test (Neville, 2005) gives two important parameters. The
first is known as first crack strength, which is primarily controlled by the matrix. The
second is known as the ultimate flexural strength or the modulus of rapture, which is
determined by the maximum load that can be attained. Rectangular beams were used
for this test using the two point loading arrangement specified in the Test method BS
1881-Part 118, 1983. While the test was conducted, the development of first crack
and the cracking up to the failure was closely observed. Record the maximum
reading showed at the display before the specimen failed and measure the distance
from the crack to the nearest support. Figure 3.12 shows the flexural test machine.

33












Figure 3.12: Flexural test machine




3.7.3 Splitting Tensile Test


In this test concrete (Neville, 2005) cylinder is placed with its axis horizontal
between the platens of a testing machine as shown in Figure 3.13. And the load is
increased until failure by indirect tension in the form of splitting along the vertical
diameter takes place. During a splitting test, the platens of testing machine should not
be allowed to rotate in a plane perpendicular to the axis of cylinder, but a slight
movement in the vertical plane containing the axis should be permitted in order to
accommodate a possible non-parallelism of the generatrices of the cylinder. This can
be achieved by means of a simple roller arrangement interposed between one platen
and the cylinder. The rate of loading is prescribed by BS 1881: Part 117: 1983.






34











Figure 3.13: Concrete cylinder after testing for tension




3.8 Thermogravimetric (TG) Analysis


Thermogravimetric analysis (TGA) is a technique which examines the mass
change of a sample as a function of temperature. TGA data were analyzed by
obtaining the first derivative of the resulting pattern. The first derivative provides a
better tool for defining and attributing the weight loss to different phases. It is
expected that ettringite, monosulfate, and the corresponding carbonated phases
(carboaluminate, hemicarboaluminate, and monocarboaluminate) could all exist
within the paste of investigated specimens. Quantification of AFt and AFm phases
was not done individually, but as a whole in the temperature range from 50C to 260
C. TG analysis allows the estimation of the content of Ca(OH)
2
from the weight
losses in the range of temperatures from 400 550
o
C and quantified based on the
limits of the first derivative of the resulting peaks. The analysis was carried out on
powdered samples using Mettler TG50 system. Samples were heated over the range
of 40 900
o
C at a constant rate of 20
o
C/min in N
2
atmosphere. TG analysis was
carried out to determine the relative amount of Ca(OH)
2
in the concrete samples
prepared.

35


3.9 Microstructural Analysis


The structural development of cement is a result of complex hydration
reactions that stiffens, densify and impart structural integrity on the product (Conner,
1990). The main hydration phases under normal conditions are C-S-H gel of
variable stoichiometry and calcium hydroxide which together form about 90 % (w/w)
of the solid hydration products in an OPC paste. The other solid hydration products
are hexacalcium aluminoferrite trisulfate or ettringite type phases and tetracalcium
aluminate monosulfate or monosulfate.


Field emission scanning electron microscopy (FESEM) was used to observe
the morphology of the POFA and concrete samples. Samples that were tested for
strength were soaked in acetone and stored in desiccators until examined. Samples
were manually fractured mounted onto aluminum stubs using conductive carbon
coated cement double sided tape. Samples were coated with gold-palladium for
microstructural scanning. All samples were kept in desiccator prior to analysis.


In the presence of POFA, pozzolanic reaction occurs , involving the reaction
between calcium hydroxide with SiO
2
or Al
2
O
3
-SiO
2
framework to form calcium
silicate hydrate, calcium aluminate hydrate and calcium aluminate ferrite hydrate.
The main reaction product of pozzolanic reaction is C-S-H gel that enhanced the
strength of cement (James and Rao, 1986). Hydration processes that result in
densification of the cement matrix can improve the ability of the product to combat
aggressive condition.






36




CHAPTER IV




RESULTS AND DISCUSSION




4.1 Introduction


In this chapter, various tests conducted on the specimens will be looked into.
The present study aims to investigate the workability, compressive strength, and
flexural strength, and indirect tensile strength of palm oil fuel ash concrete. The
specimens were cured and tested at ages that explained in the previous chapter. Palm
oil fuel ash is added based on the percentage of cement content. Also, the
information may be very useful for future study and future development of building
materials. All the test methods were done as described in chapter III of this thesis.




4.2 Slump Test Results


Figure 4.1 shows the results of slump test. It can be seen that the slump value
for the control mix P0 is not within the design range which is 30 mm-60 mm because
of the effect of using superplasticizer. It can be seen that POFA concrete exhibit
37

lower value of slump compared to slump of OPC concrete. It was also observed that
among POFA results, the finer the POFA, the lower the slump.


When using POFA 10 m, concrete in both replacement percentages 20 %
and 30 % exhibit lower workability. In contrast, by using POFA 45 m concrete
exhibits higher workability. For the same fineness of POFA, it is evident that by
replacing OPC by 30 % of POFA it will result in higher workability than using 20 %
replacement.



80
40
35
75
65
0
10
20
30
40
50
60
70
80
90
P0 P1 P2 P3 P4
Mi x
S
l
u
m
p

(
m
m
)










Figure 4.1: Slump test results


The high demand for water as the ash content increases is due to increased
amount of silica in the mixture. This is typical of pozzolan cement concrete as the
silica-lime reaction requires more water in addition to water required during
hydration of cement (Adesanya and Raheem, 2009). As the natural pozzolan addition
ratio increased, water demand to obtain the same consistency and workability
increases. The reason for this is that the rate of increase of water demand is not as
high as the natural pozzolan addition ratio can be, so that natural pozzolan is finely
divided and has a lubricant effect on concrete (Yetgin and Ahmet, 2006).

38

4.3 Compacting Factor Results


The results of the compaction factor test can be correlated to slump. Figure
4.2 shows higher degree of compaction for the control mix P0 compared to POFA
concrete. Not only that, but also among mixes with POFA results i.e. P1, P2, P3, and
P4; at the higher percentage of replacement concrete exhibit lower slump and
consequently, lower degree of compaction.












Figure 4.2: compacting factor results
0.95
0.93
0.96
0.95
0.97
0.91
0.92
0.93
0.94
0.95
0.96
0.97
0.98
P0 P1 P2 P3 P4
Mi x
C
o
m
p
a
c
t
i
n
g

f
a
c
t
o
r

Figure 4.2: Compacting Factor Results




4.4 Compressive Strength


As described in chapter III, total of 75 cube specimens with the size of 100
x100 x 100 mm were tested for compressive strength for P
0
, P
1
, P
2
, P
3
, and P
4
. The
specimens were tested at 7, 28, and 90 days after curing in water. Table 4.1 shows
the compressive strength results for these mixes. Specimens were tested for
39

compressive strength by applying increasing compressive load until failure occurs.
Thus, reading of the maximum load for failure can be obtained. The calculation for
compressive strength is obtained from the following equation:

Compressive Strength = P/A

Where:
P: Ultimate compressive load of concrete (N)
A: Surface area in contact with the platens (mm
2
)



Figure 4.3 shows the relationship between compressive strength results. It can
be seen that, among POFA concrete compressive strength results, the higher
compressive strength was achieved when using OPC replaced with 20 % of 10 m
POFA. Although the higher compressive strength achieved is 58.05 MPa when using
POFA, but it can be seen that this strength did not exceed the compressive strength
for the control mix P
0
when using OPC only. This is because of the lower percentage
of superplasticizer used. The low percentage of superplasticizer will result in lower
compressive strength at early ages. And as a result, the quantity of calcium hydroxide
Ca(OH)
2
will be less, and as a consequence, less C-S-H gel which plays an
important role in making more dense concrete when reacting with the silica
contained in the POFA. (Mahmud, 1996) and (Awal, 1998) observed that by
incorporating superplasticizer, remarkable achievements in the development of
strength have been shown to occur in POFA concrete. And the superplasticizer
increases not only the early-age strength but also increases the long-term
development of concrete strength.







40

Table 4.1: Compressive strength results

Mix 7-days compressive
strength (MPa)
28-days compressive
strength (MPa)
90-days compressive
strength (MPa)
P
0
48.73 59.8 66.3
P
1
39.70 46.45 58.05
P
2
34.55 46.06 46.65
P
3
34.89 45.41 50.52
P
4
29.45 41.37 45.10














4
8
.
7
3
3
9
.
7
0
3
4
.
5
5
3
4
.
8
9
2
9
.
4
5
5
9
.
8
4
6
.
4
5
4
6
.
0
6
4
5
.
4
1
4
1
.
3
7
6
6
.
3
5
8
.
0
5
4
6
.
6
5
5
0
.
5
2
4
5
.
1
0
10
20
30
40
50
60
70
80
P0 P1 P2 P3 P4
C
o
m
p
r
e
s
i
o
n

S
t
r
e
n
g
t
h

(
M
P
a
)
Mix
7 days
28 days
90 days

Figure 4.3: Relationship between compressive strength results





41

4.5 Flexural Strength Results


As described in chapter III, total of 15 specimens of rectangular beams with
the size of 500 mm in length, 100 mm in width and 100 mm in thickness were tested
for observing POFA concrete in flexural behavior, see Table 3.2. The specimens
were tested at 28 days after curing in water. Specimens were tested for flexural
strength by applying increasing load until failure occurs. Thus, reading of the
maximum load for failure can be obtained. The calculation for flexural strength or
the modulus of rapture, which is determined by the maximum load, is obtained from
the following equation (Neville, 2005):


Modulus of rapture (MoR), f
b
(N/mm
2
) =
3
bd
PL
if
3
L
a > (4.1)


Where,
P = maximum load
L = span of beam (400 mm)
b = width of beam
d = depth of beam
a = position of fracture from near support



The results at 28-day of flexural strength for all specimens tested are shown
in Figure 4.4. It can be observed that the flexural strength of POFA is slightly lower
than that of OPC. By comparing results among POFA concrete, it is found that by
using 30 % of 45 m POFA gave a higher flexural strength. At the same time, it is
much closer to that of OPC concrete. It also can be seen that by using higher
percentage of POFA which is 30 %, a higher flexural strength was achieved.


42








7.95
7.57
7.68
7.5
7.83
7
7.2
7.4
7.6
7.8
8
8.2
P0 P1 P2 P3 P4
F
l
e
x
u
r
a
l

s
t
r
e
n
g
t
h

(
M
P
a
)
Mix






Figure 4.4: Flexural Strength Results




4.6 Splitting Tensile Test Results


Total of 25 cylinders were tested for tensile at 28 days for mixes where
shown in Table 3.2. Figure 4.5 shows splitting tensile strength results for these
mixes. It can be seen that the behavior of concrete in tension is nearly the same to the
behavior in flexure. Except for P
2
and P
4
show convergent strength results. Although
the results of POFA concrete in tension are different but alike. The higher percentage
of replacement of P2 and P4 when using 30 % POFA gave results of tensile quite the
same. In general, POFA concrete is lesser than OPC concrete in tension.






43



9.04
6.72
8.08
7.77
8.14
0
2
4
6
8
10
12
P0 P1 P2 P3 P4
T
e
n
s
i
l
e

S
t
r
e
n
g
t
h

(
M
P
a
)
Mix














Figure 4.5: Splitting tensile strength results




4.7 Chemical Analysis of POFA and OPC


The single point BET surface area for POFA10 m and POFA 45 m is 47
and 28 m
2
/g, respectively. POFA of 10 m showed a higher surface area as expected
due to its smaller particle size compared to POFA 45. The higher surface area for
POFA 10 m could result in a higher rate of reaction, hence higher compressive
strength. Samples containing 20 % of POFA 10 m and 30 % of POFA 10 m,
showed higher compression strength compared to the samples containing POFA 45
m at 90 days curing age.


Both physical properties and chemical analysis indicated that POFA is a
pozzolanic material (Awal and Hussin, 1997; Sumadi and Hussin, 1993). This
pozzolanic material is grouped in between Class C and Class F as specified in
ASTMC618-92a (Awal and Hussin, 1997). POFA is moderately rich in silica content
meanwhile lime content is very low as compared to OPC (Awal and Hussin, 1997).
However, the chemical composition of POFA can be varied due to operating system
in palm oil mill. Table (4.2) shows the chemical composition of the OPC and POFA.
44

Table 4.2: Chemical composition of OPC and POFA

Chemical Composition POFA OPC
Silica (SiO
2
) 48.99 21.45
Aluminium Oxide (Al
2
O
3
) 3.78 3.62
Ferric Oxide (Fe
2
O
3
) 4.89 3.50
Calcium Oxide (CaO) 11.69 60.98
Magnesium Oxide (MgO) 1.22 0.59
Sodium Oxide (Na
2
O) 0.73 0.25
Potassium Oxide (K
2
O) 4.01 0.51
Magnesium Oxide (MnO
3
) 0.01 0.25
Loss on Ignition (LOI) 10.51 1.37
















4.8 Thermogravimetric Analysis ( TGA)


Thermogravimetry and differential thermogravimetry analysis of the concrete
samples containing POFA 10 m, (P
1
and P
2
), and the other one containing POFA 45
m; (P
3
and P
4
) at 90 days curing age, and which were cured in water showed that
the weight loss due to dehydroxylation of Ca(OH)
2
occurred between 410
o
C to
470
o
C. Significant weight loss between 550
o
C and 750
o
C is also was observed. At
temperatures above 550
o
C weight loss is attributed partially to CO
2
from
decomposition of CaCO
3
and partially due to the final stages of dehydration of C-S-
H and the hydrated aluminate phases (Taylor, 1990). Some researches attributed
weight losses between 650
o
C and 850
o
C as being due to the decomposition of CaCO
3

to CO
2
and CaO (Pacewska, et al., 2002). Table 4.3 shows the percent weight losses
for P
1
, P
2
, P
3
and P
4
at 7, 28 and 90- day curing ages.







45

Table 4.3: The percent weight loss for P
1
, P
2
, P
3
, and P
4

Sample Percentage of weight loss %
7 Days 28 Days 90 Days
P
1
0.46 0.71 0.87
P
2
0.70 0.73 0.77
P
3
1.125 0.92 0.43
P
4
1.11 0.91 0.50



Based on the percent weight loss attributed to dehydroxylation of calcium
hydroxide, Ca(OH)
2
or portlandite, the amount of Ca(OH)
2
increases with curing age
for P1 indicating the progress of cement hydration reaction. For P
2
samples there is
no increase in strength for 28-day and 90-day samples. The percent weight loss
attributed to dehydroxylation of calcium hydroxide remained unchanged for this
sample at the said curing ages. For P
3
and P
4
, a reduction in weight loss attributed to
dehydroxylation of calcium hydroxide, or portlandite and subsequent increase in
compression is indicative of pozzolanic reaction. This higher strength can be
attributed to the pozzolanic reaction which occurred between the silica in POFA and
calcium hydroxide which results from the cement hydration reaction. Table 4.4
showed the percent weight loss and temperature ranges for P
0
, P
1
, P
2
, P
3,
and P
4
at
90- day curing ages.



Table 4.4: Thermogravimetry data for Po, P1, P2, P3 and P4 at 90 days curing age


Sample
Temperature ranges for weight loss and percent
weight loss (%)
50 - 250C
o
C 410 470
o
C
P
0
5.8 1.85
P
1
7.5 0.87
P
2
6.7 0.77
P
3
8.2 0.43
P
4
10 0.5











46

AFt and AFm phases in the temperature range from 50C to 260C shows
that all samples exhibit weight loss in this temperature range with P4 having the
highest weight loss (10%).




4.9 Microstructural Analysis (FESEM)


The structural development of cement is a result of complex hydration
reactions that stiffens, densify and impart structural integrity on the product (Conner,
1990). The main hydration phases under normal conditions are C-S-H gel of
variable stoichiometry and calcium hydroxide which together form about 90 % (w/w)
of the solid hydration products in an OPC paste. The other solid hydration products
are hexacalcium aluminoferrite trisulfate or ettringite type phases and tetracalcium
aluminate monosulfate or monosulfate.


In the presence of POFA, pozzolanic reaction occurs , involving the reaction
between calcium hydroxide with SiO
2
or Al
2
O
3
-SiO
2
framework to form calcium
silicate hydrate, calcium aluminate hydrate and calcium aluminate ferrite hydrate.
The main reaction product of pozzolanic reaction is C-S-H gel that enhanced the
strength of cement (James and Rao, 1986). Hydration processes that result in
densification of the cement matrix can improve the ability of the product to combat
aggressive condition.


In this study the microstructure of P
0
, P
1
, P
2
, P
3
and P
4
were studied using
Field Emission Scanning Electron Microscope (FESEM) at 3 and 7-day curing ages.
A porous morphology is observed at 1000X magnfication at 3-day curing age as can
be seen in Figure 4.6. At higher magnification, granules of POFA were observed and
also the occurrence of typical hydration reaction products is observable in the
samples that are shown in Figure 4.7.
47















Figure 4.6: FESEM of P
4
at 3 days using 1000X magnification showing
porous morphology.
















Figure 4.7: Granules of POFA when using 1000 X magnification of P
3
at 3
days
48

Radiating clusters of Type I C-S-H gel could be observed distributed in all
the samples. Radiating clusters of C-S-H will eventually lead to a densification the
structure, and an increase in strength. Figure 4.8 show higher magnification of
sample P
3,
it can be seen the presence of fine needle like structures of ettringite
crystals. Studies have shown that the superplasticizer accelerate early ettringite
formation as well as producing ettringite crystals which are smaller. Hexagonal
platelets of Ca(OH)
2
could be observed in some samples as shown in Figure 4.9.
Hexagonal platelets of Ca(OH)
2
are less evidence. Figure 4.10 and Figure 4.11 show
the FESEM of P
3
at 3 and 7 days at three different magnifications which is 500,
1000, and 2000 X.



















Figure 4.8: FESEM of P
3
at 7 days using 2000X magnification





49
















Figure 4.9: FESEM, P
2
at 7 days, hexagonal platelets of Ca(OH)
2.






















50
















































Figure 4.10: Microstructure of P
3
at 3 days at 500, 1000, and 2000 X magnification



51














































Figure 4.11: Microstructure of P
3
at 7 days at 500, 1000, and 2000 X magnification






52

4.10 Summary


This chapter represents the characteristics features of palm oil fuel ash used
and its influence on some properties of fresh and hardened concrete. Properties of
ash obtained in this present research suggest that POFA is a good pozzolanic material
due to its higher content of silica compared to that of OPC.


Test on workability behavior of concrete containing POFA did not show any
satisfactory result. It has observed that by inclusion the POFA in concrete, the
workability was reduced.


The factors that are responsible for the development of strength of concrete
with common pozzolanic materials have shown to influence the strength of concrete
containing palm oil fuel ash. Study on the effect of using more fine ash with different
contents on compressive strength revealed that, because of pozzolanic activity and
higher surface area, it is better to replace 20 % of cement by POFA of 10 m rather
than using POFA of 30 m with both 20 % and 30 % replacement that is because of
the higher surface area when using POFA of 10 m. Although the results of strength
in flexure and tensile are different but alike. The replacement of OPC with POFA has
result in lower tensile strength. On the other hand, among POFA concrete results, the
higher the replacement the higher the tensile strength. Tests on flexural strength have
revealed to the same of flexural strength.


Studies on samples using Field Emission Scanning Electron Microscope
(FESEM) at 3 and 7-days curing ages revealed that, occurrence of typical hydration
reaction products is observable.




53






CHAPTER V




CONCLUSIONS AND RECOMMENDATIONS
FOR FUTURE STUDY




5.1 Introduction


Although conclusions in the form of summary have been mentioned at the
ends of the previous chapters, a short account of important research findings making
up resolutions is presented here for the sake of clarity.




5.2 Behavior of POFA Concrete in the Fresh State


POFA concrete exhibit lower value of slump compared to slump of OPC
concrete. It was also observed that among POFA results, the finer the POFA the
lower the slump. The results of the compaction factor test can be correlated to the
slump. The higher the percentage of replacement concrete exhibit lower slump and
consequently, lower the degree of compaction.

54

5.3 Behavior of POFA Concrete in the Hardened State


Study on the effect of using more fine ash with different contents on
compressive strength revealed that, because of pozzolanic activity and higher surface
area, it is better to replace 20 % of cement by POFA of 10 m rather than using
POFA of 30 m with both 20 % and 30 % replacement that is because of the higher
surface area when using POFA of 10 m. The flexural strength of POFA is slightly
lower than that of OPC. Like that of flexural strength, tensile strength of concrete
containing POFA developed in the similar way.




5.4 Thermogravimetric analysis (TGA)


Thermogravimetry analysis of the concrete samples containing POFA
revealed that, the amount of Ca(OH)
2
increases with curing age indicating the
progress of cement hydration reaction. Reduction in weight loss attributed to
dehydroxylation of calcium hydroxide, or portlandite and subsequent increase in
compression is indicative of pozzolanic reaction.




5.5 Microstructural Analysis (FESEM)


A porous morphology is observed in some samples at 1000X magnification
and radiating clusters of C-S-H will lead to a densification the structure, and an
increase in strength. Hexagonal platelets of Ca(OH)
2
could be observed in some
samples and they are less evidence in relation to the strength.

55

5.6 Recommendations for Future Investigation


a. If concepts were developed, it would not be necessarily mean that this
will remain true for all the time. The properties of the ash may vary
from source of supply to another depending on the type of the raw
material and efficiency of burning.

b. Manufacture and testing of concrete with various mix proportions are
recommended not only to satisfy the individual need but also to find a
broader perspective on behavior of this new pozzolanic material.

c. The effect of superplasticizer was observed to be very significant not
only on the early-age strength but also on the development of late-age
strength. Consequently trial mix on different content of
superplasticizer is strongly recommended.

d. Previous researches have revealed that incorporation of POFA in
concrete is advantageous for the durability of concrete in: the rise of
heat, carbonation, penetration of chloride ions, and sulphate
environment. At the same time, using POFA in concrete as
replacement materials, limited compressive strength of 60 MPa was
achieved. Contribution of POFA with high cementitious material such
as GGBFS to get high strength high performance concrete is mainly
recommended.










56

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