binder characterization and performance of...

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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

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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.

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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

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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

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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

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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

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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


5.2 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

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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


6.2 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

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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


7.2 Conclusions 256

7.3 Recommendations 259

REFERENCES 260

Appendix A 277

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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

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used (penetration) 112


used (softening point) 115

4.5 G*/sin δ at failure temperature 119


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

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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

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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



4.5 Penetration 110

4.6 Softening point 113

4.7 Viscosity 116

4.8 G*/sin δ versus temperature for WCO 1 sample 118



4.11 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


treated WCO (un-aged) 149

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untreated WCO (aged) 151


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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