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1
BINDER CHARACTERIZATION AND PERFORMANCE OF ASPHALTIC
CONCRETE MODIFIED WITH WASTE COOKING OIL
WAN NUR AIFA BT. WAN AZAHAR
UNIVERSITI TEKNOLOGI MALAYSIA
5
BINDER CHARACTERIZATION AND PERFORMANCE OF ASPHALTIC
CONCRETE MODIFIED WITH WASTE COOKING OIL
WAN NUR AIFA BT. WAN AZAHAR
A thesis submitted in partial fulfilment of the
requirements for the award of the degree of
Doctor of Philosophy (Civil Engineering)
Faculty of Civil Engineering
Universiti Teknologi Malaysia
MARCH 2018
iii
DEDICATION
“To my beloved parents, siblings and friends who are always behind and
supporting me”
iv
ACKNOWLEDGEMENT
First of all, I would like to express my highest gratitude to Allah s.w.t for
granting me the opportunity to complete my PhD research for the award of the
degree of Doctor of Philosophy (Civil Engineering).
Besides, I would like to express my deep appreciation to my supervisor, Dr.
Ramadhansyah Putra Jaya for the continuous support, supervision, critical comments
and guidance throughout this year in completing my thesis project. His motivation,
enthusiasm and immense knowledge has inspired me to work hard in order to finish
my research. My appreciation also goes to my Co-supervisor, Prof. Dr. Mohd Rosli
Hainin and Dr. Norzita Ngadi for their encouragements, efforts and excellent advices
in helping me to improve the thesis.
In addition, my thanks are forwarded to all the technicians in Highway and
Transportation Laboratory of Universiti Teknologi Malaysia for their assistance and
cooperation during my laboratory works. Last but not least, I would like to thank
everyone especially my parents, siblings and friends who were involved directly or
indirectly in this research. Thanks again from bottom of my heart.
Wan Nur Aifa bt. Wan Azahar
2018
v
ABSTRACT
The use of waste cooking oil (WCO) in binder modification is widely
explored in response to waste management issue. However, the decreasing
rheological performance pattern trend at high temperature by using WCO is globally
recorded and yet still unresolved. This poor performance is due to the high acidity of
the WCO. To resolve this issue, a chemical treatment was proposed to reduce the
acidity of the WCO. Therefore, the aim of this study was to evaluate the performance
of binders modified with untreated and treated WCO. It was carried out in three
phases. In Phase 1, the physical and rheological tests of binder (penetration,
softening point, viscosity and DSR) were conducted to determine the optimum
percentages of untreated and treated WCO (between 0, 5, 10, 15 and 20%) in
modifying the binder. In Phase 2, the optimums WCOs were utilised for further
mechanical performance evaluation of Asphaltic Concrete 14 (AC14) mixture
through Marshall stability, resilient modulus, dynamic creep and indirect tensile
strength (ITS). The morphology and microstructure observations were performed in
Phase 3 to investigate the adhesion bonding between modified binder and aggregates.
The test results showed that the acidity of the WCO decreased after chemical
treatment. The rheological test showed that the failure temperature of binder
modified using the treated WCO has increased to 70 oC. In addition, treated WCO
mixture recorded superior performance by being less susceptible to permanent
deformation as compared to the control mix. Besides, the microstructure analysis
revealed that low surface roughness of binder modified with treated WCO has
strengthened the adhesion bonding with aggregates. In conclusion, the chemical
treatment had improved the treated WCO performance in the modified binder as
asphalt paving materials.
vi
ABSTRAK
Penggunaan sisa minyak masak (WCO) dalam pengubahsuaian pengikat
diterokai secara meluas sebagai respon kepada isu pengurusan sisa. Namun,
penurunan pola corak prestasi reologi pada suhu tinggi dengan menggunakan WCO
telah direkodkan secara global dan masih belum diselesaikan lagi. Prestasi lemah ini
disebabkan oleh keasidan WCO yang tinggi. Untuk menyelesaikan isu ini, rawatan
kimia dicadangkan untuk mengurangkan keasidan WCO. Oleh itu, matlamat kajian
ini adalah untuk menilai prestasi pengikat diubahsuai dengan WCO yang tidak
dirawat dan dirawat. Ianya dijalankan dalam tiga fasa. Fasa pertama, ujian fizikal dan
reologi untuk pengikat (penusukan, titik lembut, kelikatan dan reometer ricih
dinamik) dijalankan untuk menentukan peratusan optimum WCO yang tidak dirawat
dan dirawat (antara 0, 5, 10, 15 dan 20%) dalam mengubahsuai pengikat. Fasa kedua,
optimum WCO digunakan untuk penilaian prestasi mekanikal campuran asfalt
konkrit 14 (AC14) melalui kestabilan Marshall, modulus kebingkasan, rayapan
dinamik dan kekuatan tegangan tidak langsung (ITS). Pemerhatian morfologi dan
mikrostruktur dilakukan dalam fasa ketiga untuk menyiasat ikatan lekatan antara
pengikat diubahsuai dan agregat. Keputusan ujian menunjukkan keasidan WCO
menurun selepas rawatan kimia. Ujian reologi menunjukkan suhu kegagalan untuk
pengikat diubahsuai menggunakan WCO dirawat telah meningkat kepada 70 oC.
Tambahan, campuran WCO dirawat merekodkan prestasi lebih baik yang kurang
terdedah kepada ubah bentuk kekal berbanding campuran kawalan. Selain itu,
analisis mikrostruktur mendedahkan kekasaran permukaan rendah oleh pengikat
diubahsuai dengan WCO dirawat memperkuatkan ikatan lekatan dengan agregat.
Kesimpulannya, rawatan kimia meningkatkan prestasi WCO dirawat dalam pengikat
diubahsuai sebagai bahan turapan asfalt.
vii
TABLE OF CONTENTS
CHAPTER TITLE PAGE
DECLARATION ii
DEDICATION iii
ACKNOWLEDGEMENT iv
ABSTRACT v
ABSTRAK vi
TABLE OF CONTENTS vii
LIST OF TABLES xiv
LIST OF FIGURES xvii
LIST OF ABBREVIATIONS xxii
LIST OF SYMBOLS xxivv
LIST OF APPENDICES xxvi
1 INTRODUCTION 1
1.1 Background of the Study 1
1.2 Problem Statement 4
1.3 Aim and Objectives of the Study 6
1.4 Scope of the Work 6
1.5 Significance of Study 8
1.6 Summary 9
2 LITERATURE REVIEW 11
2.1 Introduction 11
2.2 Asphalt Binder 12
viii
2.2.1 The Characteristic of Binder 12
2.3 Asphalt Binder Modification 14
2.4 Waste Cooking Oil (WCO) 16
2.5 Characterisation of WCO 18
2.5.1 Chemical Properties 18
2.5.2 Physiochemical Properties 20
2.6 Chemical Reaction During Frying 22
2.6.1 Hydrolytic Reactions 22
2.6.2 Oxidative Reactions 23
2.6.3 Thermolytic Reactions 25
2.7 Physical and Chemical Changes in WCO 26
2.8 Application of WCO in Previous Study 29
2.8.1 Recyclability of WCO as a Modifier
for Binder Modification 29
2.8.2 Microstructure Observation of WCO
in Modified Binder 36
2.8.3 Asphalt Mixture Evaluation 37
2.8.4 Discussion on Previous Research 39
2.9 Problems Associated with WCO Usage 41
2.10 Factors Affecting to the Performance of WCO
in Modified Binder 42
2.10.1 Chemical Compatibility 42
2.10.2 WCO Quality 43
2.11 Proposed Potential Solution 45
2.12 Hot Mix Asphalt (HMA) 50
2.13 Rutting or Permanent Deformation 51
2.14 Summary 53
3 RESEARCH METHODOLOGY 55
3.1 Introduction 55
3.2 Phase 1: Performance Evaluation of Modified
Binder with WCO 57
3.2.1 Binder Properties 57
3.2.2 Waste Cooking Oil (WCO) 57
ix
3.2.3 Preliminary Test 59
3.2.3.1 Acidity Test 59
3.2.3.2 Water Content Test 61
3.2.3.3 Antioxidant Component
through Determination of
Aging Rate 61
3.2.4 Transesterification Process 62
3.2.5 Preparation of Modified Binder with
the WCO 65
3.2.6 Penetration Test 66
3.2.7 Softening Point Test 66
3.2.8 Viscosity Test 66
3.2.9 Dynamic Shear Rheometer (DSR)
Test 67
3.2.10 Temperature Susceptibility of Binder 68
3.2.10.1 Penetration-Viscosity
Number (PVN) 69
3.2.11 Rolling Thin Film Oven (RTFO) Test 71
3.3 Phase 2: Performance Evaluation of Asphalt
Mixture 71
3.3.1 Aggregates Properties 72
3.3.2 Sieve Analysis of Coarse and Fine
Aggregate 72
3.3.3 Mineral Filler 73
3.3.4 Aggregate Gradation 73
3.3.5 Specific Gravity 75
3.3.6 Aggregate Impact Value (AIV) Test 75
3.3.7 Aggregate Crushing Value (ACV)
Test 76
3.3.8 Flakiness Index (FI) Test 76
3.3.9 Elongation Index (EI) Test 77
3.3.10 Marshall Design Method 77
3.3.11 Theoretical Maximum Density
(TMD) 78
x
3.3.12 Resilient Modulus (MR) Test 79
3.3.13 Dynamic Creep Test 82
3.3.14 Indirect Tensile Strength (ITS) Test 85
3.4 Phase 3: Morphology and Microstructure
Analysis 86
3.4.1 Mechanical Theory 87
3.4.1.1 Atomic Force Microscopy
(AFM) Test 87
3.4.2 Chemical Theory 91
3.4.2.1 Gas Chromatography-Flame
Ionisation Detection (GC-
FID) Test 93
3.4.2.2 Gas Chromatography-Mass
Spectrometry (GC-MS) Test 94
3.4.2.3 Fourier Transform Infrared
(FTIR) Test 95
3.4.3 Field Emission Scanning Electron
Microscope (FESEM) Test 97
3.4.4 X-Ray Diffraction (XRD) Test 99
3.5 Summary 101
4 PRELIMINARY TEST AND BINDER
EVALUATION 102
4.1 Introduction 102
4.2 Preliminary Test 103
4.2.1 WCO Quality Parameter 103
4.2.1.1 Acidity 103
4.2.1.2 Water Content 105
4.2.1.3 Antioxidant Content through
Aging Index Measurement 106
4.2.2 Penetration 109
4.2.3 Softening Point 112
4.2.4 Viscosity 115
4.2.5 Rutting Resistance (G*/sin δ) 117
xi
4.2.6 Summary of Preliminary Test 121
4.3 Pre-treatment of WCO 122
4.4 Physiochemical Properties of Untreated and
Treated WCO 122
4.5 Binder Evaluation for Physical and Rheological
Performance 124
4.5.1 Penetration 124
4.5.2 Softening Point 129
4.5.3 Viscosity 134
4.5.4 Rutting Resistance (G*/sin δ) 139
4.5.5 Relationship Between Complex
Modulus (G*) and Phase Angle (δ) 147
4.5.6 Failure Temperature 153
4.5.7 Penetration-Viscosity Number (PVN) 157
4.5.8 Determination of An Optimum
Modified Binder Percentage
Containing Untreated and Treated
WCO 161
4.6 Summary 162
5 MECHANICAL PERFORMANCE OF HOT MIX
ASPHALT 163
5.1 Introduction 163
5.2 Aggregates Properties 164
5.2.1 Specific Gravity (SG) 164
5.2.2 Water Absorption (WA) 165
5.2.3 Aggregate Impact Value (AIV) 166
5.2.4 Aggregate Crushing Value (ACV) 166
5.2.5 Flakiness Index (FI) 167
5.2.6 Elongation Index (EI) 168
5.3 Marshall Mix Design 168
5.3.1 Volumetric Properties, Marshall
Stability and Flow 168
5.3.1.1 Density 169
xii
5.3.1.2 Voids Filled with Bitumen
(VFB) 171
5.3.1.3 Voids in Total Mix (VTM) 174
5.3.1.4 Stability 177
5.3.1.5 Flow 180
5.3.1.6 Stiffness 183
5.3.2 Determination of Optimum Bitumen
Content (OBC) 185
5.4 Resilient Modulus (MR) 187
5.4.1 Total Recoverable Horizontal
Deformation δ (µm) 191
5.5 Dynamic Creep 195
5.5.1 Relationship Between Cumulative
Strain and Time of Loading 199
5.6 Indirect Tensile Strength (ITS) 206
5.7 Summary 209
6 MORPHOLOGY AND MICROSTRUCTURE
OBSERVATION 211
6.1 Introduction 211
6.2 Atomic Force Microscopy (AFM) 212
6.3 Gas Chromatography-Mass Spectrometry (GC-
MS) 221
6.4 Fourier Transform Infrared (FTIR) 227
6.4.1 Control Binder 227
6.4.2 Modified Binder with Untreated
WCO 229
6.4.3 Modified Binder with Treated WCO 231
6.5 Mechanism of Adhesion Between Binder-
Aggregates Based on Chemical Composition 235
6.6 Field Emission Scanning Electron Microscope
(FESEM) 238
6.6.1 Control Mixture 238
6.6.2 Untreated WCO Mixture 240
xiii
6.6.3 Treated WCO Mixture 242
6.7 X-Ray Diffraction (XRD) 246
6.7.1 Control Binder 246
6.7.2 Modified Binder with Untreated
WCO 248
6.7.3 Modified Binder with Treated WCO 250
6.8 Summary 253
7 CONCLUSIONS AND RECOMMENDATIONS 255
7.1 Introduction 255
7.2 Conclusions 256
7.3 Recommendations 259
REFERENCES 260
Appendix A 277
xiv
LIST OF TABLES
TABLE NO. TITLE PAGE
2.1 Free fatty acids in waste cooking oil 18
2.2 FFA composition in fresh and waste cooking oil
(Maneerung et al., 2016) 20
2.3 Physiochemical properties of unused and used
cooking oil (Ullah et al., 2014) 21
2.4 Nonrecoverable creep compliance (Jnr) results
(Wen et al., 2013) 33
2.5 CSED results at low temperature (Wen et al., 2013) 38
2.6 Comparison of various methods for
transesterification (Leung et al., 2010) 48
2.7 Recommended FFA for alkali catalysts
transesterification 49
3.1 Gradation limits of the combined aggregates for
AC 14 74
3.2 AC14 mix requirement based on JKR (2008)
specification 78
3.3 Resilient modulus test parameter 80
3.4 The example of polar and non-polar in polarity
group (www.columbia.edu) 92
4.1 Acidity in WCO 104
4.2 One way ANOVA for various WCO content
(penetration) 112
4.3 One way ANOVA for different qualities of WCO
xv
used (penetration) 112
4.4 One way ANOVA for different qualities of WCO
used (softening point) 115
4.5 G*/sin δ at failure temperature 119
4.6 One way ANOVA for different qualities of WCO
used (failure temperature) 120
4.7 Physiochemical properties of untreated and treated
WCO 124
4.8 One way ANOVA for penetration (untreated
WCO) 129
4.9 One way ANOVA for penetration (treated WCO) 129
4.10 One way ANOVA for softening point (untreated
WCO) 134
4.11 One way ANOVA for softening point (treated
WCO) 134
4.12 Viscosity result for untreated WCO 137
4.13 Viscosity result for treated WCO 137
4.14 G*/sin δ at failure temperature for un-aged sample 141
4.15 G*/sin δ at failure temperature for aged sample 145
4.16 One way ANOVA for G*/sin δ (untreated WCO) 147
4.17 One way ANOVA for G*/sin δ (treated WCO) 147
4.18 One way ANOVA for failure temperature
(untreated WCO) 157
4.19 One way ANOVA for failure temperature (treated
WCO) 157
4.20 Penetration-viscosity number (PVN) for untreated
WCO 160
4.21 Penetration-viscosity number (PVN) for treated
WCO 160
4.22 Summary of the bitumen properties 161
5.1 Specific gravity result 165
5.2 Water absorption result 165
5.3 Aggregate impact value result 166
5.4 Aggregate crushing value result 167
xvi
5.5 Flakiness index result 167
5.6 Elongation index result 168
5.7 Marshall result and specifications at OBC value 187
5.8 The independent samples t-test for resilient modulus 191
5.9 The independent samples t-test for recoverable
deformation 195
5.10 The independent samples t-test for creep stiffness 199
5.11 Coefficients of linear relationship between
cumulative strain and time of loading for primary
and secondary zones at 40 °C 202
5.12 Coefficients of linear relationship between
cumulative strain and time of loading for primary
and secondary zones at 60 °C 205
5.13 One way ANOVA for indirect tensile strength
(ITS) 209
6.1 Chemical composition for control binder (60/70) 222
6.2 FFA components in WCO 223
6.3 Chemical composition for modified binder with
5% untreated WCO 224
6.4 Chemical composition for modified binder with
5% treated WCO 226
xvii
LIST OF FIGURES
FIGURE NO. TITLE PAGE
2.1 The dependency of binder properties on temperature
(McGennis et al., 1995) 13
2.2 The viscoelastic behaviour of binder (McGennis
et al., 1995) 14
2.3 Oil sample after frying process 16
2.4 Thermal oxidation reactions in oil (Choe and Min,
2007) 24
2.5 The formation of polymerisation reactions (Choe and
Min, 2007) 26
2.6 Degradation of WCO quality parameter (Choe and
Min, 2007) 27
2.7 G*.sin δ versus WCO percentage (Maharaj et al., 2015) 31
2.8 G*/sin δ versus WCO percentage (Maharaj et al., 2015 31
2.9 G*.sin δ versus temperature (Maharaj et al., 2015) 32
2.10 G*/sin δ versus temperature (Maharaj et al., 2015) 32
2.11 Rutting parameter (G*/sin δ) versus temperature for
unaged sample (Al-Omari et al., 2018) 34
2.12 Effect of WVO percentage on m-value (Al-Omari
et al., 2018) 35
2.13 Effect of temperature at different percentage of biodiesel
by-product from WCO on the stiffness (Sun et al., 2015) 35
2.14 Functional groups in control binder (Sun et al., 2015) 36
2.15 Functional groups in biodiesel by-product from WCO
xviii
(Sun et al., 2015) 37
2.16 Flow number at different percentage of bio-asphalt
from WCO (Wen et al., 2013) 38
2.17 Schematic diagram of the rutting process (Kandhal
and Cooley Jr., 2003) 52
3.1 Experimental framework 56
3.2 Filtered waste cooking oil 58
3.3 Titration process before (a) and after (b) 60
3.4 Karl-Fischer (KF) coulometer for water content test 61
3.5 Reaction during transesterification process 63
3.6 Transesterification process 64
3.7 Separation of the by-products 64
3.8 Untreated WCO (left) and treated WCO (right) 64
3.9 Mixing process for untreated and treated WCO in
modified binder 65
3.10 Dynamic shear rheometer (DSR) apparatus 68
3.11 A chart for the determination of PVN (McLeod, 1976) 70
3.12 Aggregate gradation for AC 14 74
3.13 Theoretical maximum density (TMD) apparatus 79
3.14 Set up of mixture sample for resilient modulus test 81
3.15 Set up of mixture sample for dynamic creep test 83
3.16 Relationship between permanent strain and number of
loading cycles (Zhao, 2002) 85
3.17 AFM equipment 88
3.18 Principle of AFM (De Oliviera et al., 2012) 89
3.19 Sample preparation for AFM test 90
3.20 Example of non-contact mode (De Oliviera et al.,
2012) 90
3.21 Gas chromatography – flame ionisation detection
(GC-FID) equipment 93
3.22 The operation system in flame-ionisation detection
(FID) (fid-principles
http://www.cambustion.com/products/hfr500) 94
xix
3.23 Gas chromatography – mass spectrometry (GC-MS)
equipment 95
3.24 FTIR equipment 96
3.25 Schematic diagram of FTIR operation (Shimadzu
FTIR IRTracer – 100) 97
3.26 FESEM equipment 98
3.27 Detecting system in FESEM (Hitachi UHR FESEM) 99
3.28 XRD equipment 100
3.29 Diffraction in XRD (X-ray diffraction: web.pdx.edu) 101
4.1 Water content 106
4.2 Aging index for WCO 1 107
4.3 Aging index for WCO 2 107
4.4 Aging index for WCO 3 107
4.5 Penetration 110
4.6 Softening point 113
4.7 Viscosity 116
4.8 G*/sin δ versus temperature for WCO 1 sample 118
4.9 G*/sin δ versus temperature for WCO 2 sample 118
4.10 G*/sin δ versus temperature for WCO 3 sample 118
4.11 Penetration for untreated and treated WCO 126
4.12 Softening point for untreated and treated WCO 131
4.13 Determination of mixing and compaction temperature 138
4.14 Rutting performance of WCO at untreated condition
(unaged) 140
4.15 Rutting performance of WCO at treated condition
(unaged) 140
4.16 Rutting performance of WCO at untreated condition
(aged) 144
4.17 Rutting performance of WCO at treated condition
(aged) 144
4.18 Complex modulus (G*) and phase angle (δ) for
untreated WCO (un-aged) 148
4.19 Complex modulus (G*) and phase angle (δ) for
treated WCO (un-aged) 149
xx
4.20 Complex modulus (G*) and phase angle (δ) for
untreated WCO (aged) 151
4.21 Complex modulus (G*) and phase angle (δ) for
treated WCO (aged) 151
4.22 Failure temperature at un-aged and aged condition 155
5.1 The density of AC 14 170
5.2 The VFB of AC 14 172
5.3 The VTM of AC 14 176
5.4 The stability of AC 14 178
5.5 The flow of AC 14 181
5.6 The stiffness of AC 14 183
5.7 Resilient modulus 188
5.8 Recoverable horizontal deformation 192
5.9 Dynamic creep stiffness 196
5.10 Cumulative strain at 40 oC 201
5.11 Cumulative strain at 60 oC 204
5.12 Indirect tensile strength (ITS) 207
6.1 Summarised of AFM images 214
6.2 Detailed AFM images of control binder 218
6.3 Detailed AFM images of modified binder with
untreated WCO 219
6.4 Detailed AFM images of modified binder with treated
WCO 220
6.5 Transesterification process 225
6.6 Functional group from FTIR analysis for control
binder (60/70) 228
6.7 Functional group from FTIR analysis for modified
binder with 5% untreated WCO 230
6.8 Functional group from FTIR analysis for modified
binder with 5% treated WCO 233
6.9 The trends of functional group from FTIR analysis for
control and modified binder 234
6.10 Illustration of adhesion bonding mechanism between
binder-aggregates 237
xxi
6.11 FESEM image for control mixture 239
6.12 Elemental composition in control mixture 240
6.13 FESEM image for 5% untreated WCO mixture 241
6.14 Elemental composition in 5% untreated WCO mixture 242
6.15 FESEM image for 5% treated WCO mixture 243
6.16 Elemental composition in 5% treated WCO mixture 245
6.17 XRD graph pattern for control binder (60/70) 247
6.18 XRD graph pattern for modified binder with untreated
WCO 249
6.19 XRD graph pattern for modified binder with treated
WCO 252
xxii
LIST OF ABBREVIATIONS
AC 14 - Asphaltic concrete of nominal maximum aggregate size 14 mm
AFM - Atomic force microscopy
AI - Aging index
Al - Aluminum
ANOVA - Analysis of Variance
ASTM - American Society for Testing Materials
BBR - Bending beam rheometer
COD - Chemical oxygen demand
CSED - Critical strain energy density
DSR - Dynamic shear rheometer
EDX - Energy dispersive x-ray spectroscopy
Fe - Iron
FESEM - Field emission scanning electron microscope
FFA - Free fatty acid
FTIR - Fourier transform infrared
GCMS - Gas chromatography-mass spectrometry
HMA - Hot Mix Asphalt
ITS - Indirect tensile strength
ITSM - Indirect tensile stiffness modulus
JKR - Jabatan Kerja Raya
K - Potassium
KOH - Potassium hydroxide
LVDT - Linear Variable Displacement Transducer
MSCR - Multiple stress creep and recovery
NaOH - Sodium hydroxide
xxiii
OBC - Optimum bitumen content
PVN - Penetration viscosity number
RTFO - Rolling thin film oven
TMD - Theoretical maximum density
USD - Universal sorption device
UTM - Universiti Teknologi Malaysia
UVO - Used vegetable oil
VFB - Voids filled with bitumen
VTM - Voids in total mix
WCO - Waste cooking oil
WMA - Warm mix asphalt
WVO - Waste vegetable oil
XRD - X-ray diffraction
xxiv
LIST OF SYMBOLS
c - y-intercept
oC - Celsius
cm - centimetre
cm-1 - reciprocal wavelength
cm3 - cubic centimetre
cP - centiPoise
cSt - centiStokes
dmm - decimillimetre
oF - Fahrenheit
g - gram
G* - complex modulus
h - hour
Hz - Hertz
J - Joules
Jnr - Nonrecoverable creep compliance
kg - kilogram
km - kilometre
kPa - kilo Pascal
kv - kilovolt
m - slope
m3 - cubic metre
meq - miliequivalents
mg - milligram
ml - millilitre
mm - millimetre
xxv
mm2 - millimetre square
µm - micrometre
MPa - Mega Pascal
MR - Resilient modulus
N - Newton
N KOH - Molarity KOH
nm - nanometre
Pa.s - Pascal seconds
R2 - Regression
rpm - revolution per minute
s - second
% - percentage
δ - Delta/phase angle
σ - applied stress
ɛ - recoverable strain
xxvi
LIST OF APPENDICES
APPENDIX TITLE PAGE
A List of Publications 277
1
CHAPTER 1
INTRODUCTION
1.1 Background of the Study
Petroleum-based asphalt binder is derived from petroleum refinement process
by-product (Wen et al., 2013). Bitumen is recognised as an essential coating material
in bituminous pavements composition apart from the aggregates skeleton for
pavement construction. In asphalt mixture composition, the binder functions as an
adhesive agent for coating process and binds the aggregate particles together.
Generally, pure bitumen production through crude oil petroleum refining process is
not desirable in road pavement application. The asphalt binder exhibits insufficient
properties for pavement construction and need to be modified with various additives
types such as carbonaceous materials, fine minerals and polymers (Chebil et al.,
2000). An improvement of engineering properties for asphalt binder can be achieved
with the application of a modifier by reducing temperature susceptibility and
enhancing the rheological performance to withstand the environmental and traffic
loading. Currently, a number of notable studies are being conducted worldwide to
explore valuable resources from waste materials as a modifier for asphalt binder
modification.
2
In recent years, a wide range of oil-based modifications have been
introduced, especially involving waste cooking oil (WCO). The WCO is also
recognised as waste grease oil which is characterised as the by-product of fresh
cooking oil produced during cooking and food processing. This oil source has
recently gained widespread attention because of its satisfactory achievement as a
potential waste material to enhance the physical and rheological performance of
modified binder. The oil undergoes three types of common chemical reaction during
frying, such as hydrolysis, oxidation and polymerisation. The chemical process in oil
causes degradation in the physical and chemical properties (Cvengroš and
Cvengrošová, 2004) which affects WCO quality. Physical properties include
alteration in foaming quantity, colour, viscosity, density and flavour. Meanwhile
chemical properties are represented as total unsaturation compound, free fatty acid
content, polar and polymeric material. The generation of huge quantities of WCO is
attributed by the increasing human population and its use as a frequent medium for
food preparation involving frying. It can be noticed that WCO production quantity is
directly proportional to frying rate.
According to Chhetri et al. (2008), enormous quantity of WCO that is
generated worldwide is illegally dumped and released into the surrounding
environment. In Malaysia, the disposal of WCO is reported to be approximately
around 50,000 tons, which was produced from plant and animal based fats source
(Yaakob et al., 2013). These wastes are disposed to the environment without
undergoing any proper treatment (Kheang et al., 2006). A survey conducted by
Kabir et al. (2014) revealed that the majority of the respondents (54.5%) discard
WCO into their house sink. Meanwhile 22.2% stated that the WCO is dumped into
drains. This coincides with the response on the level of awareness on WCO
recycling. Unexpectedly, only 12% of the households WCO is recycled, while most
of the respondents (about 88%) did not practice waste recycling as they discharge
WCO improperly. Such inappropriate action has consequently induced an
undesirable impact to the entire environmental ecosystem, for instance distraction of
aquatic life, contamination of water and soil, sewer system blockage and increased
maintenance cost for water treatment and waste management (Chen et al., 2009).
3
Abundant of WCO production can cause prominent adverse impact and threat
to the environment if not properly managed and disposed. Therefore, recycling or
reusing WCO in modified asphalt binder is considered as an effective utilisation and
management of this waste while at the same time ensuring economic and
environmental benefits (Patil et al., 2012). It is noteworthy that, most researchers
have focused on the superior performance of WCO as a rejuvenator for aged binder
(Asli and Karim, 2011; Zargar et al., 2012; Asli et al., 2012; Zaumanis et al., 2013;
Chen et al., 2014a; Binbin et al., 2014; Chen et al., 2014b), apart from substituting
WCO in modified binder to improve rheological performance. The WCO
performance as a modifier at high and low temperatures was evaluated by Wen et al.
(2013). The rheological findings indicate declination of the complex modulus (G*),
which resulted in a low rutting resistance at high temperature. On the contrary, an
increment in thermal cracking resistance performance at low-temperature was
observed to occur linearly with the addition of WCO content.
This rheological result coincides with the study conducted by Maharaj et al.
(2015) for un-aged sample, wherein an enhancement of fatigue cracking resistance
was achieved at low temperature. Meanwhile, the high temperature performance
showed an adverse effect as the rutting resistance decreased with the addition of
WCO. This is also supported by Sun et al. (2016), which reveals the decrement of
deformation resistance and improvement of thermal cracking resistance performance
when using the modified binder incorporated with bio-oil derived from WCO.
According to Teymourpour et al. (2015), the application of WCO in conventional
binder proved an enhancement of thermal cracking resistance but compromising the
high temperature performance as evidenced by the reduction of resistance to rutting.
The superiority performance of fatigue cracking resistance was noticeable with the
addition of WCO as reported in a previous research. It proves that the capability of
WCO to improve low temperature performance, while deteriorating the rutting
resistance performance at high temperature.
The WCO in asphalt binder softens the physical properties of modified
asphalt binder, thereby unable to withstand rutting exposure. According to Katamine
4
(2000), the negative indicator in the quality of bitumen is expected with the addition
of WCO in bitumen. This serves as the major reason why WCO is not suggested for
optimal utilisation, due to its poor performance in rutting resistance, which is not
desirable especially for hot climatic region. Owing to the adverse and unsatisfactory
performance in rheological properties, no further research work was conducted to
evaluate the mechanical properties of asphalt mixture. This is due to the expectation
of high tendency for rutting problem, thereby reducing the strength of asphalt
mixture. Waste oil needs to be fully re-evaluated and assessed by undergoing further
treatment before being recommended and applied in the asphalt binder to produce
bituminous mixture (Borhan et al., 2009).
However, despite the broadly practiced WCO application, the identification
of fundamental parameters influencing WCO in binder modification and also the
effectiveness of the process has not been investigated yet (Teymourpour et al., 2015).
In addition, the mechanism for modifying asphalt binder with WCO and the effect of
WCO on the modified binder performance are not clearly documented. Obviously,
the softer and less viscous modified binder with WCO depicts the weakness of
internal chemical bonding of the material. Hence, there is the issue of chemical
compatibility and interprets an assumption of incompatibility between these two
materials due to chemical properties that should be further clarified and investigated.
1.2 Problem Statement
A high amount of WCO is generated due to abundant fresh cooking oil
consumption during frying. Inappropriate waste disposal and dumping into the
landfill has induced an adverse impact to the surrounding environmental ecosystem.
Therefore, a waste management strategy arises to mitigate environmental pollution
due to the large quantity of WCO. Apart from waste disposal, waste utilisation has
become a valuable option due to the realisation on the significance of awareness
5
level for environmental preservation. Essentially, it is highly recommended to adopt
a more sustainable approach of recycling WCO product in modified asphalt binder as
a pavement material in road construction. The application of WCO in asphalt binder
indicates an effective solution of waste management which is gaining extensive
interest from other researchers.
Most of the previous studies have concentrated on the modified binder
incorporated with WCO (Wen et al., 2013; Maharaj et al., 2015). However, none of
the researchers emphasised on the basic parameter affecting oil modification
(Teymourpour et al., 2015). In addition, this parameter is not clearly explained since
the modification of asphalt binder with WCO is still in the empirical stage. Yet,
WCO is directly used in modified asphalt binder without determining the quality of
WCO. Theoretically, with regard to the modified binder performance, the rheological
evaluation is affected by the quality of WCO, in which the acid value is represented
as one of the main parameters for quality measurement specifically. Preliminary
finding has revealed that an increased acid value has caused the decreasing pattern
trend in rheological performance and vice versa. The increment in acid value is
attributed to the degradation rate of WCO during frying and exhibits undesirable
characteristic that constraint the optimisation of WCO in asphalt binder. Therefore,
there is an urgency for WCO to undergo a chemical pre-treatment in minimising the
existing high acid value before being utilised for the modification of asphalt binder.
It is noteworthy to compare the performance of modified binder containing untreated
and treated WCO, and identify any rheological and mechanical performance
improvement after conducting the chemical modification.
In addition, the softer and less viscous modified binder with WCO is
noticeable and hinders the application of WCO in high temperature region due to
high rutting exposure. These poor properties depict the weakness in the internal
chemical bonding and portray the disturbance of molecule particle structure of the
material. It gives an assumption that there is a restrictive factor influencing the
refusal of molecule interaction to form strong chemical bonding in the modified
asphalt binder with WCO. Therefore, the issue of chemical compatibility between
6
WCO and asphalt binder arises and should be investigated (Gong et al., 2016). Since
there is no previous research conducted to investigate the compatibility issue, there is
a need to conduct a chemical analysis in order to characterise the chemical
compatibility properties between these two materials in this study. This factor
contributes to the main reason as to why the level of WCO usage is comparatively
very low, and implies that there is a requirement to evaluate the suitability of WCO
as a modifier, which is available at low cost feedstock without compromising the
quality performance of modified binder with WCO as paving materials.
1.3 Aim and Objectives of the Study
This study aims to evaluate an asphalt mixture incorporating untreated and
treated WCO in modified binder. In order to achieve this aim, the study is carried
out to fulfil the following objectives:
1. To determine the properties of untreated and treated WCO in modified binder
for physical and rheological performance.
2. To evaluate the mechanical performance of Hot Mix Asphalt (HMA)
incorporating untreated and treated WCO.
3. To analyse the morphology and microstructure characteristics of modified
binder and asphalt mix containing untreated and treated WCO.
1.4 Scope of the Work
The scope of this research is to enhance binder properties with the upgraded
of WCO quality as a modifier through chemical treatment. The improved mechanical
7
performance exhibited by asphalt mixture incorporating treated WCO is expected to
be more superior and comparable to the conventional asphalt mixtures. Raw WCO
derived from palm oil was collected from a café surrounding UTM, Skudai. The
aggregates sample source was obtained from Hanson Quarry in Kulai, Johor. The
control asphalt binder used in this study was PEN 60/70 which was sourced from
Chevron Company and has met all the specifications as outlined by the Jabatan Kerja
Raya (2008) specifications.
The basic test for binder evaluation was performed which included
penetration test, softening point test, viscosity and dynamic shear rheometer (DSR).
The modified asphalt binder containing untreated and treated WCO underwent an
aging condition by conducting a rolling thin film oven (RTFO) only, which is
restricted for the assessment of rutting resistance at high temperature, and does not
address the fatigue cracking performance. This implies that this research is focused
on the rutting resistance performance since poor performance was recorded by the
previous work that should be improved in this study.
An optimum WCO percentage was selected based on binder evaluation for
further mechanical performance testing of asphalt mixture. The asphalt mixtures
were evaluated based on the Marshall Stability and flow test, resilient modulus test,
dynamic creep test and indirect tensile strength test. The control mixture, untreated
WCO mixture and treated WCO mixture, were compared in order to identify any
mechanical performance improvement. The microstructure observation was
conducted by using Atomic Force Microscopy (AFM), Gas Chromatography-Mass
Spectrometry (GCMS), Fourier Transform Infrared (FTIR), Field Emission Scanning
Electron Microscope (FESEM) and X-Ray Diffraction (XRD). Most of the chemical
treatment of WCO, asphalt binder and bituminous mixtures testing and
microstructure analysis were performed at the Chemical Laboratory, Transportation
and Highway Laboratory and Central Laboratory at UTM Skudai, Johor.
8
1.5 Significance of Study
WCO is identified as a valuable potential waste material that has capability to
enhance the performance of conventional asphalt binder for road pavement
construction. The superior physical and chemical properties exhibited by WCO
source attribute to the selection of this waste to be applied as a modifier in the
modification of asphalt binder. WCO can give adverse impact if not properly
managed and disposed. On the contrary, an effective management of this waste, by
recycling WCO in modified asphalt binder for paving materials, significantly
contributes to the advantages in three principles, such as environmental, economic,
and social.
From an environmental stand point, the utilisation of abundant WCO by
recycling this waste into paving materials is seen as an efficient sustainable effort
which minimises the generation of waste dumping in the landfill and illegal waste
disposal into the drainage system, reduces the consumption of natural resource and
preserves the environmental ecosystem as well. When WCO is discharged into the
river, the formation of a thin oil layer on the water surface attributes to the blockage
of sunlight energy source to pass through, that is required by the marine
environment. In addition, the presence of WCO in the water system causes the
alteration of oxygenation process by disrupting oxygen supply to the aqua marine
ecosystem. The increment of chemical oxygen demand (COD) due to WCO
existence causes water contamination in the presence of poisonous compound thus
destroying aquatic life. Meanwhile, for residential area, WCO accumulation has
induced drainage system blockage thus causing clogging problem, which in turn
increases the maintenance cost to fix and monitor this issue. Obviously, by recycling
WCO, it can mitigate and solve the environmental problem directly.
From an economical point of view, the cost of road construction may be
minimised by the usage of WCO as modifier. WCO is selected because of its low-
cost feedstock to be obtained and available abundantly (Villanueva et al., 2008).
9
Despite the cheap price, the upgraded WCO properties by chemical modification
exhibit better rheological and mechanical performance for asphalt mixture. In
comparison to other highly cost modifiers, WCO source has the capability to deliver
high performance potential as compared to other modifiers. Sustained utilisation of
WCO as a modifier in binder will be able to drastically reduce the waste disposal of
enormous WCO quantity.
The recyclability of WCO for paving material in pavement construction
industry has proved an attempt to raise awareness among Malaysian in increasing the
WCO management practice, thus improving the quality of social life based on the
social standpoint. However, this practice is still at an initial stage. Therefore, it is
necessary to empower public awareness campaign to encourage household toward
proper WCO management. The awareness campaign should briefly cover the
negative impact of inappropriate disposal of WCO and emphasise the significance of
WCO recycling for environmental benefits as well. In implementing this valuable
awareness, support from the government is required to ensure successful WCO
recycling programmes. The government should encourage citizens and industries
through advertisement and provide additional information that would be helpful in
improving the WCO recycling management.
1.6 Summary
The deficiency of the rutting resistance performance exhibited by modified
binder and asphalt mixture when dealing with oil-based source can be solved by the
improvement of untreated WCO properties through chemical modification. A
comparison on the performance of binder and asphalt mix incorporating untreated
and treated WCO, which has not been previously studied, is explored in this
research. In this regard, the study consists of three types of evaluation in terms of
binder (penetration, softening point, viscosity and DSR), mechanical asphalt mixture
260
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