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MECHANICAL AND SURFACE FREE ENERGY CHARACTERIZATION OF ASPHALT CONCRETE FOR MOISTURE DAMAGE DETECTION BY IBRAHIM M. A. ABUAWAD DISSERTATION Submitted in partial fulfillment of the requirements for the degree of Doctor of Philosophy in Civil Engineering in the Graduate College of the University of Illinois at Urbana-Champaign, 2016 Urbana, Illinois Doctoral Committee: Professor Imad Al-Qadi, Chair Professor William Buttlar Professor John Harvey Professor Emeritus Marshall Thompson Research Assistant Professor Hasan Ozer

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Page 1: MECHANICAL AND SURFACE FREE ENERGY …

MECHANICAL AND SURFACE FREE ENERGY CHARACTERIZATION OF

ASPHALT CONCRETE FOR MOISTURE DAMAGE DETECTION

BY

IBRAHIM M. A. ABUAWAD

DISSERTATION

Submitted in partial fulfillment of the requirements

for the degree of Doctor of Philosophy in Civil Engineering

in the Graduate College of the

University of Illinois at Urbana-Champaign, 2016

Urbana, Illinois

Doctoral Committee:

Professor Imad Al-Qadi, Chair

Professor William Buttlar

Professor John Harvey

Professor Emeritus Marshall Thompson

Research Assistant Professor Hasan Ozer

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ii

ABSTRACT

Moisture damage is defined as the degradation of the mechanical properties of asphalt concrete

(AC) caused by moisture. Moisture damage causes a severe loss in the strength and durability of

asphalt pavements, leading to a major decrease in pavement performance. Hence, many additives

are used to mitigate the effect of moisture on AC.

The moisture sensitivity of AC depends on many factors, including aggregates, binders, and AC

properties, environmental conditions (e.g., temperature and humidity), traffic loading, quality of

construction, and pavement design. Many laboratory tests have been developed to understand and

evaluate moisture damage. Laboratory tests are conducted at two levels, AC mixture and its

components (binder and aggregate), using various conditioning procedures to introduce the effects

of moisture.

Current AC moisture susceptibility identification laboratory tests have three main drawbacks:

limited ability of simulating environmental conditions, dependence of results on test conditioning

process, and limited correlation between laboratory and field results. These shortcomings have

compelled the need for the development of new tools to study moisture damage; especially at the

component level.

The main objective of this study is to predict the impact of several additives/modifiers and recycled

asphalt pavement (RAP) on moisture susceptibility of AC at the mixture- and component-level.

The impact was evaluated under different aging and conditioning levels. In addition, an assessment

of the impact was performed within mixture-level tests and between mixture- and component-level

tests.

The study is focused primarily on investigating the effects of moisture on AC mixtures. Two AC

mixes (in addition to selected additives and modifiers), typically used in the State of Illinois, were

considered: 19.0-mm nominal maximum aggregate size (NMAS) binder mix and 19.0-mm NMAS

mix with 50% RAP. The additives and modifiers consist of liquid anti-strip (LAS), hydrated lime

(HL), styrene butadiene styrene (SBS), SBS with LAS, and polyphosphoric acid (PPA) with HL.

The effects of the additives and modifiers on the moisture susceptibility of the proposed AC

mixtures were evaluated through several mixture- and component-level tests. The mixture-level

tests are the modified AASHTO T-283 and dynamic modulus tests. The surface free energy (SFE),

direct adhesion test (DAT) and blister test (BT) represent the component-level types.

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Samples for the mixture-level tests were prepared at different aging and conditioning durations.

Aging durations include one hour and four hours after mixing and prior to compaction;

conditioning durations comprise one thawing cycle, three freezing and thawing (FT) cycles, and

five FT cycles. Aging was also being considered at the component level by using the rolling thin

film oven (RTFO) and pressure aging vessel (PAV). Each binder was tested at the virgin, RTFO,

and PAV aging status.

The results from modified AASHTO T-283 test indicate that LAS and HL improved moisture

resistance. RAP and modified mixes (mixes with SBS or with PPA+HL) were not efficient in

reducing moisture susceptibility. Analyzing modified AASHTO T-283 results can be best

evaluated using the modified Lottman test, if extensive conditioning is considered, at four hours

aging with five FT cycles conditioning. Master curve obtained from the dynamic modulus test

found to be not as effective as tensile strength for evaluating moisture damage in AC mixes. The

improvement of AC with LAS and RAP is decreased with aging while AC with HL improvement

increased with aging.

Aggregate had higher SFE than asphalt binder. It was found that AC mixes with LAS, HL and

RAP produced the best performance considering moisture resistance when added to asphalt binder.

PPA and SBS modifiers produced insignificant alteration of control asphalt binder SFE. Results

from the SFE test suggest that there is no unique relation between SFE parameters (SFE, work of

adhesion, and work of cohesion) and aging. Direct adhesion test (DAT) appears to be incapable of

capturing aging impact on adhesion performance and unreliable in ranking and classifying asphalt

binders. This could be related to the drawbacks in sample preparation, repeatability, and sample

failure. The current blister test (BT) setup needs improvement to be able to properly assess the

adhesion characteristics of asphalt binder.

The comparison of a component level parameter (SFE) with mixture-level parameter, tensile stress

ration (TSR), showed that TSR and SFE are efficient in identifying the impact of additives on the

moisture susceptibility of AC mixes and asphalt binders. However, dynamic modulus (E*) Ratio

appears to have a potential for qualitatively evaluating moisture damage of AC mixes at excessive

conditioning. This study found that adding LAS or HL are effective in reducing moisture

susceptibility of AC mixtures.

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To Randa, Mohammad, Leen, Mom, Dad and My Family

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ACKNOWLEDGMENTS

First and for most all praises are due to my God Allah (SWT) the most Gracious and the most

Merciful for the blessings and bounties He showered upon me throughout my PhD study journey.

It is without no doubt that I could not reach this level without His care and guidance. O’ Allah

(SWT) give me the strength and ability to praise and worship you in the way you love and deserve.

Definitely, You have the complete power and Provide the best reward.

I would like to express my sincere gratitude and appreciation to Professor Imad Al-Qadi my

supervisor and mentor. The effort and time provided by Professor Al-Qadi was essential and

valuable to reach to this level. He has been guiding, supporting, and encouraging me throughout

the course of this project. In addition to his supervision, Professor Al-Qadi was kind enough to

treat me as his young brother standing beside me and generously providing me with his valuable

advices throughout my life. I am honestly so proud, thrilled and honored that I worked for him and

was able to share with him this experience which benefited me on both levels technically and

personally.

I would like to extend my deep appreciation to the members of the doctoral committee: Professors

William Buttlar, Marshall Thompson, Hasan Ozer, and John Harvey for their valuable comments

and insightful advice throughout my research. Special thanks also for Mr. Bill Pine for all the effort

and time he spent especially his assistance in finalizing the asphalt mix designs using the Bailey

method.

My sincere thanks to the professional research engineers; Jeff Kern, Jim Meister and Aaron

Coenen. Their expertise, time, and effort was very essential in making sure that the lab work was

conducted in a professional and accurate manner.

Special thanks and gratitude are extended to all my colleagues whose thoughtful discussions in our

group meetings had contributed greatly to my education and the quality of my research. Thanks to

them also for the time we spent together in which we shared our lives, experiences and cultures

especially in our monthly gathering. Special thanks for Dr. Qazi Aurangzeb and Dr. Hasan Ozer

and their families for being such good friends. Special thanks also for Mohammad Sawalha and

Rebekah Yang for their help in arranging the necessary setup for the final defense.

I would like also to acknowledge all my community brothers and their families for sharing with us

all our moments throughout our life at Urbana Champaign. I would like to specially acknowledge

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Anwar Al-Khaldi, Izzat Al-Haj, Nabil Hirz Allah, Ahmad Taha, Abdel-Kareem Saadah, Mosab

Jaradah and Ashraf Edkedek.

I owe the most to my parents and parents-in-laws, especially who traveled overseas, for their love,

support, and understanding in the course of my Ph.D. studies. Definitely special thanks to Randa

my wife, the love of my life, for her passion, love and support. Thanks to my sweetheart daughter

Leen for shinning my life. Finally, I would like to thank my beloved son Mohammad. You are the

dearest to my heart and my first joy. Please forgive me for not being there for you always, promise

I will make it up for you.

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TABLE OF CONTENTS

List of Tables ................................................................................................................................. xi

List of Figures ............................................................................................................................... xv

List of Symbols .......................................................................................................................... xviii

List of Abbreviations ................................................................................................................... xix

CHAPTER 1 INTRODUCTION AND OVERVIEW ................................................................. 1

1.1 Background ........................................................................................................................... 1

1.2 Mechanisms of Moisture Damage......................................................................................... 4

1.2.1 Asphalt Mixture Stripping .............................................................................................. 5

1.2.2 Binder Softening ............................................................................................................. 5

1.2.3 Aggregate Degradation ................................................................................................... 5

1.3 Laboratory Evaluation Of Moisture Damage ........................................................................ 6

1.3.1 Development of Moisture Damage Tests ....................................................................... 6

1.3.2 Classification of Moisture Damage Laboratory Tests .................................................... 8

1.3.3 Difficulties in Developing Moisture Damage Evaluation Tests ..................................... 9

1.4 Modeling ............................................................................................................................. 10

1.5 Problem Statement .............................................................................................................. 14

1.6 Objective and Scope ............................................................................................................ 15

1.7 Thesis Organization............................................................................................................. 16

CHAPTER 2 MATERIALS AND ASPHALT MIX................................................................. 22

2.1 Materials .............................................................................................................................. 22

2.1.1 Aggregate...................................................................................................................... 22

2.1.2 Asphalt Binder .............................................................................................................. 22

2.1.3 Additives/Modifiers ...................................................................................................... 22

2.2 Asphalt Mix ......................................................................................................................... 27

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CHAPTER 3 MIXTURE-LEVEL CHARACTERIZATION ................................................... 31

3.1 Introduction ......................................................................................................................... 31

3.2 Illinois Modified Lottman (AASHTO T-283) Test............................................................. 32

3.3 Modified Lottman Test ....................................................................................................... 34

3.4 Dynamic Modulus Test ....................................................................................................... 34

3.5 Aging And Conditioning ..................................................................................................... 35

CHAPTER 4 COMPONENT-LEVEL CHARACTERIZATION............................................. 39

4.1 Introduction ......................................................................................................................... 39

4.2 Materials .............................................................................................................................. 39

4.3 Adhesion Tests .................................................................................................................... 39

4.3.1 Surface Free Energy ..................................................................................................... 40

4.3.2 Direct Adhesion Test .................................................................................................... 44

4.3.3 Blister Test .................................................................................................................... 45

CHAPTER 5 MIXTURE-LEVEL TESTS: RESULTS AND DISCUSSION .......................... 50

5.1 Introduction ........................................................................................................................ 50

5.2 Results and discussion ........................................................................................................ 51

5.2.1 Illinois Modified Lottman Test (AASHTO T 283) ................................................. 51

5.2.2 Modified Lottman Test (AASHTO T 283) ............................................................. 52

5.2.3 Complex Modulus (AASHTO T 342) .................................................................... 56

5.3 Summary ............................................................................................................................ 59

CHAPTER 6 COMPONENT-LEVEL TESTS: RESULTS AND DISCUSSION.................... 93

6.1 Preface ................................................................................................................................ 93

6.2 Results And Discussion ...................................................................................................... 93

6.2.1 Surface Free Energy ................................................................................................ 93

6.2.2 Direct Adhesion Test ............................................................................................ 102

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6.2.3 Blister Test ............................................................................................................ 104

6.3 Summary .......................................................................................................................... 104

CHAPTER 7 MIXTURE AND COMPONENT LEVEL RELATIONSHIP .......................... 118

7.1 Introduction ...................................................................................................................... 118

7.2 Dynamic modulus ratio .................................................................................................... 118

7.3 Modified AASHTO vs. Dynamic Modulus ..................................................................... 119

7.3.1 1 hr short-term aging and IDOT conditioning ...................................................... 119

7.3.2 1 hr short-term aging and 3 FT conditioning ........................................................ 119

7.3.3 1 hr short-term aging and 5 FT conditioning ........................................................ 120

7.3.4 4 hrs short-term aging and IDOT conditioning ..................................................... 120

7.3.5 4 hrs short-term aging and 3 FT conditioning ...................................................... 121

7.3.6 4 hrs short-term aging and 5 FT conditioning ...................................................... 121

7.4 SFE vs. mixture-level tests ............................................................................................... 123

7.5 Summary .......................................................................................................................... 127

CHAPTER 8 SUMMARY, CONCLUSION AND RECOMMENDATIONS ....................... 140

8.1 Findings ............................................................................................................................. 140

8.1.1 Modified Lottman Test (AASHTO T 283) ................................................................. 141

8.1.2 Complex Modulus (AASHTO T 342) ........................................................................ 142

8.1.3 Surface Free Energy ................................................................................................... 142

8.1.4 Direct Adhesion Test .................................................................................................. 143

8.1.5 Blister Test .................................................................................................................. 143

8.1.6 Mixture-Level Tests Correlation ................................................................................ 143

8.1.7 Mixture and Component-Level Tests Correlation ...................................................... 144

8.2 Conclusions ....................................................................................................................... 144

8.3 Impact of The Study .......................................................................................................... 145

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8.4 Recommendations ............................................................................................................. 145

REFERENCES ........................................................................................................................... 147

APPENDIX A: SURFACE FREE ENERGY DETAILED MEASUREMENTS ...................... 164

APPENDIX B: E* RATIO DETAILED CALCULATIONS ..................................................... 166

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LIST OF TABLES

Table 2.1 Main Features of Aggregates: (a) Gradations (b) Aggregate Physical Properties ........ 29

Table 2.2 N90 Control Mix Designs ............................................................................................. 30

Table 2.3 Mix Design of All N90 Mixes ...................................................................................... 30

Table 2.4 RAP Mix Design ........................................................................................................... 30

Table 5.1. Moisture Susceptibility Evaluation for N90 Control Mix ........................................... 86

Table 5.2 IDT Strength Results for Asphalt Mixes at Different Aging and Conditioning Periods

....................................................................................................................................................... 86

Table 5.3 TSR Values for Asphalt Mixes at Different Aging and Conditioning Periods ............ 87

Table 5.4 Statistical Analysis for IDT (psi) of Control Mixes ..................................................... 88

Table 5.5 Statistical Analysis for IDT (psi) Tests of Mixes with LAS ......................................... 88

Table 5.6 Statistical Analysis for IDT (psi) Tests of Mixes with LAS ......................................... 88

Table 5.7 Statistical Analysis for IDT (psi) Tests of Mixes with PPA+HL ................................. 89

Table 5.8 Statistical Analysis for IDT (psi) Tests of Mixes with SBS ......................................... 89

Table 5.9 Statistical Analysis for IDT (psi) Tests of Mixes with SBS+LAS ............................... 90

Table 5.10 Statistical Analysis for IDT (psi) Tests of Mixes with RAP ...................................... 90

Table 5.11 Statistical Analysis for TSR (%) of Control Mixes .................................................... 90

Table 5.12 Statistical Analysis for TSR (%) of Mixes with LAS ................................................. 91

Table 5.13 Statistical Analysis for TSR (%) of Mixes with HL ................................................... 91

Table 5.14 Statistical Analysis for TSR (%) of Mixes with PPA+HL ......................................... 91

Table 5.15 Statistical Analysis for TSR (%) with Mixes with SBS ............................................. 92

Table 5.16 Statistical Analysis for TSR (%) for Mixes with SBS+LAS ...................................... 92

Table 5.17 Statistical Analysis for TSR (%) of Mixes with RAP ................................................ 92

Table 6.1 SFE for Asphalt Binder and Work of Cohesion at the Virgin Level .......................... 114

Table 6.2 SFE for Asphalt Binder and Work of Cohesion at the RTFO Level .......................... 114

Table 6.3 SFE for Asphalt Binder and Work of Cohesion at the PAV Level ............................ 115

Table 6.4 SFE for aggregate ....................................................................................................... 115

Table 6.5 Work of Adhesion of Asphalt Binder with Dolomitic Limestone at the Virgin Level

..................................................................................................................................................... 115

Table 6.6 Work of Adhesion of Asphalt Binder with Dolomitic Limestone at the RTFO Level116

Table 6.7 Work of Adhesion of Asphalt Binder with Dolomitic Limestone at the PAV Level . 116

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Table 6.8 Pmax and E for Asphalt Binders at Virgin and RTFO State......................................... 117

Table 6.9 Coefficient of Variance (in Percent) for Pmax and E at Virgin and RTFO State ......... 117

Table 7.1 E* Ratio (%) for Control Asphalt Mixture after 1hr Short-term Aging (a) Dynamic

Modulus at All Conditioning Levels (b) E* Ratio Calculation .................................................. 129

Table 7.2 E* Ratio for Asphalt Mixtures after 1 hr Short-term Aging ....................................... 129

Table 7.3 E* Ratio for Asphalt Mixtures after 4 hrs Short-term Aging ..................................... 130

Table 7.4 E* Ratio (%) Statistical Analysis for Asphalt Mixes at IDOT Conditioning after 1 hr

Aging........................................................................................................................................... 130

Table 7.5 E* Ratio (%) Statistical Analysis for Asphalt Mixes at 3 FT Conditioning after 1 hr

Aging........................................................................................................................................... 130

Table 7.6 E* Ratio (%) Statistical Analysis for Asphalt Mixes at 5 FT Conditioning after 1 hr

Aging........................................................................................................................................... 131

Table 7.7 E* Ratio (%) Statistical Analysis for Asphalt Mixes at IDOT Conditioning after 4 hrs

Aging........................................................................................................................................... 131

Table 7.8 E* Ratio (%) for Statistical Analysis Asphalt Mixes at 3 FT Conditioning after 4 hrs

Aging........................................................................................................................................... 132

Table 7.9 E* Ratio (%) Statistical Analysis for Asphalt Mixes at 5 FT Conditioning after 4 hrs

Aging........................................................................................................................................... 132

Table 7.10 TSR (%) Results for Asphalt Mixes after 1 hr Aging............................................... 133

Table 7.11 TSR (%) Results for Asphalt Mixes after 4 hrs Aging ............................................. 133

Table 7.12 TSR (%) Statistical Analysis for Asphalt Mixes at IDOT Conditioning after 1 hr

Aging........................................................................................................................................... 134

Table 7.13 TSR (%) Statistical Analysis for Asphalt Mixes at 3 FT Conditioning after 1 hr Aging

..................................................................................................................................................... 134

Table 7.14 TSR (%) Statistical Analysis for Asphalt Mixes at 5 FT Conditioning after 1 hr Aging

..................................................................................................................................................... 135

Table 7.15 TSR (%) Statistical Analysis for Asphalt Mixes at IDOT Conditioning after 4 hrs

Aging........................................................................................................................................... 135

Table 7.16 TSR (%) Statistical Analysis for Asphalt Mixes at 3 FT Conditioning after 4 hrs

Aging........................................................................................................................................... 136

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Table 7.17 TSR (%) Statistical Analysis for Asphalt Mixes at 5 FT Conditioning after 4 hrs

Aging........................................................................................................................................... 136

Table 7.18 Impact of additives, modifiers, and RAP with respect to Control Mix after 1 hr aging

and adopted conditioning levels (IDOT, 3FT, and 5FT) ............................................................ 137

Table 7.19 Impact of additives, modifiers, and RAP with respect to Control Mix after 4 hrs aging

and adopted conditioning levels (IDOT, 3FT, and 5FT) ............................................................ 137

Table 7.20 E* Ratio and TSR correlation for asphalt mixes at considered aging and conditioning

levels ........................................................................................................................................... 138

Table A.1 Probe liquids total SFE and SFE components ........................................................... 164

Table A.2 Control asphalt binder contact angles with probe liquids .......................................... 164

Table A.3 Control+LAS asphalt binder contact angles with probe liquids ................................ 164

Table A.4 Control+HL asphalt binder contact angles with probe liquids .................................. 164

Table A.5 PPA+HL asphalt binder contact angles with probe liquids ....................................... 164

Table A.6 SBS asphalt binder contact angles with probe liquids ............................................... 165

Table A.7 SBS+LAS asphalt binder contact angles with probe liquids ..................................... 165

Table A.8 RAP asphalt binder contact angles with probe liquids .............................................. 165

Table A.9 Aggregate contact angles with probe liquids ............................................................. 165

Table B.1 E* Ratio for Control asphalt mixture after 1hr short-term aging (a) Dynamic modulus

at all conditioning levels (b) E* Ratio calculation ...................................................................... 166

Table B.2 E* Ratio for Control+LAS asphalt mixture after 1hr short-term aging (a) Dynamic

modulus at all conditioning levels (b) E* Ratio calculation ....................................................... 167

Table B.3 E* Ratio for Control+HL asphalt mixture after 1hr short-term aging (a) Dynamic

modulus at all conditioning levels (b) E* Ratio calculation ....................................................... 168

Table B.4 E* Ratio for PPA+HL asphalt mixture after 1hr short-term aging (a) Dynamic

modulus at all conditioning levels (b) E* Ratio calculation ....................................................... 169

Table B.5 E* Ratio for SBS asphalt mixture after 1hr short-term aging (a) Dynamic modulus at

all conditioning levels (b) E* Ratio calculation .......................................................................... 170

Table B.6 E* Ratio for SBS+LAS asphalt mixture after 1hr short-term aging (a) Dynamic

modulus at all conditioning levels (b) E* Ratio calculation ....................................................... 171

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Table B.7 E* Ratio for RAP asphalt mixture after 1hr short-term aging (a) Dynamic modulus at

all conditioning levels (b) E* Ratio calculation .......................................................................... 172

Table B.8 E* Ratio for Control asphalt mixture after 4hrs short-term aging (a) Dynamic modulus

at all conditioning levels (b) E* Ratio calculation ...................................................................... 173

Table B.9 E* Ratio for Control+LAS asphalt mixture after 4hrs short-term aging (a) Dynamic

modulus at all conditioning levels (b) E* Ratio calculation ....................................................... 174

Table B.10 E* Ratio for Control+HL asphalt mixture after 4hrs short-term aging (a) Dynamic

modulus at all conditioning levels (b) E* Ratio calculation ....................................................... 175

Table B.11 E* Ratio for PPA+HL asphalt mixture after 4hrs short-term aging (a) Dynamic

modulus at all conditioning levels (b) E* Ratio calculation ....................................................... 176

Table B.12 E* Ratio for SBS asphalt mixture after 4hrs short-term aging (a) Dynamic modulus at

all conditioning levels (b) E* Ratio calculation .......................................................................... 177

Table B.13 E* Ratio for SBS+LAS asphalt mixture after 4hrs short-term aging (a) Dynamic

modulus at all conditioning levels (b) E* Ratio calculation ....................................................... 178

Table B.14 E* Ratio for RAP asphalt mixture after 4hrs short-term aging (a) Dynamic modulus

at all conditioning levels (b) E* Ratio calculation ...................................................................... 179

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LIST OF FIGURES

Figure 1.1 Fatigue cracking, rutting, raveling and potholes captured in winter 2013/2014 in

Urbana-Champaign, IL. ................................................................................................................ 17

Figure 1.2 Effect of moisture diffusion: (a) cohesive failure and (b) adhesive failure (Kringos et

al. 2008a)....................................................................................................................................... 20

Figure 1.3 Mastic erosion caused by fast flowing water (Kringos et al. 2008a). ......................... 20

Figure 1.4 Pumping action mechanism (Kringos et al. 2008a)..................................................... 21

Figure 1.5 3D X-ray CT with imaging analysis technique (Kassem et al. 2006). ........................ 21

Figure 1.6 Finite element mesh for modeling moisture damage (Kringos et al. 2008b). ............. 21

Figure 3.1 Indirect tensile (IDT) strength testing. ........................................................................ 37

Figure 3.2 Experimental setup of dynamic modulus test. ............................................................. 37

Figure 3.3 Experimental matrix for each asphalt mix: (a) Lottman test; (b) complex modulus test.

....................................................................................................................................................... 38

Figure 4.1 Sessile drop device. ..................................................................................................... 46

Figure 4.2 Contact angle measurement. ........................................................................................ 46

Figure 4.3 SFE asphalt binder sample. ......................................................................................... 46

Figure 4.4 Aggregate SFE sample. ............................................................................................... 47

Figure 4.5 SFE-based evaluation parameters: work of adhesion (top); work of cohesion (bottom).

....................................................................................................................................................... 47

Figure 4.6 DAT specimen fixture. ................................................................................................ 48

Figure 4.7 Typical DAT results (Al-Qadi et al. 2008). ................................................................. 48

Figure 4.8 Blister sample aluminum substrate with and without asphalt binder. ......................... 48

Figure 4.9 Schematic showing blister mechanism (Al-Qadi et al. 2008). .................................... 49

Figure 5.1 Indirect tensile (IDT) strength results for asphalt mixes at different aging and

conditioning periods...................................................................................................................... 60

Figure 5.2 Tensile strength ratio (TSR) values for asphalt mixes at various aging and

conditioning periods...................................................................................................................... 60

Figure 5.3 Complex modulus for control mixes: (a) 1 hr aging; (b) 4 hrs aging .......................... 61

Figure 5.4 Complex modulus for control mixes (a) 1 hr vs 4 hrs aging at unconditioned; (b) 1 hr

vs 4 hrs aging at IDOT conditioning............................................................................................. 62

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Figure 5.5 Complex modulus for control mixes: (a) 1 hr vs 4 hrs aging at 3 FT; and (b) 1 hr vs 4

hrs aging at 5 FT ........................................................................................................................... 63

Figure 5.6 Complex modulus for mixes with LAS: (a) 1 hr aging; (b) 4 hrs aging ..................... 64

Figure 5.7 Complex modulus for mixes with LAS: (a) 1 hr vs 4 hrs aging at unconditioned; (b) 1

h vs 4 hrs aging at IDOT conditioning.......................................................................................... 65

Figure 5.8 Complex modulus for mixes with LAS: (a) 1 h vs 4 hrs aging at 3 FT; and (b) 1 hr vs

4 hrs aging at 5 FT ........................................................................................................................ 66

Figure 5.9 Complex modulus for mixes with LimeD: (a) 1 hr aging; (b) 4 hrs aging .................. 67

Figure 5.10 Complex modulus for mixes with LimeD: (c) 1 hr vs 4 hrs aging at unconditioned;

(d) 1 hr vs 4 hrs aging at IDOT conditioning ................................................................................ 68

Figure 5.11 Complex modulus for mixes with LimeD: (a) 1 hr vs 4 hrs aging at 3 FT; and (b) 1

hr vs 4 hrs aging at 5 FT ............................................................................................................... 69

Figure 5.12 Complex modulus for mixes with PPA+LimeD: (a) 1 hr aging; (b) 4 hrs aging ...... 70

Figure 5.13 Complex modulus for mixes with PPA+LimeD: (a) 1 hr vs 4 hrs aging at

unconditioned; (b) 1 hr vs 4 hrs aging at IDOT conditioning....................................................... 71

Figure 5.14 Complex modulus for mixes with PPA+LimeD: (a) 1 hr vs 4 hrs aging at 3 FT; and

(b) 1 hr vs 4 hrs aging at 5 FT ....................................................................................................... 72

Figure 5.15 Complex modulus for mixes with SBS: (a) 1 hr aging; (b) 4 hrs aging .................... 73

Figure 5.16 Complex modulus for mixes with SBS: (a) 1 hr vs 4 hrs aging at unconditioned; (b)

1 hr vs 4 hrs aging at IDOT conditioning ..................................................................................... 74

Figure 5.17 Complex modulus for mixes with SBS: (a) 1 hr vs 4 hrs aging at 3 FT; and (b) 1 hr

vs 4 hrs aging at 5 FT .................................................................................................................... 75

Figure 5.18 Complex modulus for mixes with SBS+LAS: (a) 1 hr aging; (b) 4 hrs aging .......... 76

Figure 5.19 Complex modulus for mixes with SBS+LAS: (a) 1 hr vs 4 hrs aging at

unconditioned; (b) 1 hr vs 4 hrs aging at IDOT conditioning....................................................... 77

Figure 5.20 Complex modulus for mixes with SBS+LAS: (a) 1 hr vs 4 hrs aging at 3 FT; and (b)

1 hr vs 4 hrs aging at 5 FT ............................................................................................................ 78

Figure 5.21 Complex modulus for mixes with RAP: (a) 1 hr aging; (b) 4 hrs aging ................... 79

Figure 5.22 Complex modulus for mixes with RAP: (a) 1 hr vs 4 hrs aging at unconditioned; (b)

1 hr vs 4 hrs aging at IDOT conditioning ..................................................................................... 80

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Figure 5.23 Complex modulus for mixes with RAP: (a) 1 hr vs 4 hrs aging at 3 FT; and (b) 1 hr

vs 4 hrs aging at 5 FT .................................................................................................................... 81

Figure 5.24 Complex modulus for the mixes at 1 hr aging and unconditioned ............................ 82

Figure 5.25 Complex modulus for the mixes at 4 hrs aging and unconditioned .......................... 82

Figure 5.26 Complex modulus for mixes at 1 hr aging and IDOT conditioning .......................... 83

Figure 5.27 Complex modulus for mixes at 4 hrs aging and IDOT conditioning ........................ 83

Figure 5.28 Complex modulus for mixes at 1 hr aging and 3 FT conditioning ............................ 84

Figure 5.29 Complex modulus for mixes at 4 hrs aging and 3 FT conditioning .......................... 84

Figure 5.30 Complex modulus for mixes at 1 hr aging and 5 FT conditioning ............................ 85

Figure 5.31 Complex modulus for mixes at 4 hrs aging and 5 FT conditioning .......................... 85

Figure 6.1 SFE of asphalt binder at the virgin, RTFO, and PAV aging levels. .......................... 106

Figure 6.2 Work of cohesion of asphalt binder at the virgin, RTFO, and PAV aging levels. .... 106

Figure 6.3 Work of adhesion of asphalt binder with dolomitic limestone at the virgin, RTFO, and

PAV aging levels. ....................................................................................................................... 107

Figure 6.4 Peak load (Pmax) for asphalt binders at virgin and RTFO state. ................................ 107

Figure 6.5 Bond energy (E) for asphalt binders at virgin and RTFO state. ................................ 108

Figure 6.6 Trimming the DAT sample excessive asphalt binder. ............................................... 108

Figure 6.7 Removing the shim from DAT sample prior to testing. ............................................ 109

Figure 6.8 Removing the DAT sample bottom aluminum base. ................................................ 109

Figure 6.9 Tilting failure. ............................................................................................................ 110

Figure 6.10 BT sample with smaller diameter. ........................................................................... 110

Figure 6.11 BT sample with original diameter and half-original thickness. .............................. 111

Figure 6.12 BT sample with original diameter and double original thickness. .......................... 111

Figure 6.13 No separation for BT sample with smaller diameter. .............................................. 112

Figure 6.14 No separation for BT sample with original diameter and half-original thickness. . 112

Figure 6.15 No separation for BT sample with original diameter, double original thickness, and

small orifice diameter. ................................................................................................................ 113

Figure 6.16 No separation for BT sample with original diameter, double original thickness, and

large orifice diameter. ................................................................................................................. 113

Figure 7.1 SFE results of asphalt binders for RTFO aging level. ............................................... 128

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LIST OF SYMBOLS

𝑁𝑖, 𝑁𝑗 = shape functions

𝐿 = storage coefficient

ℎ = pressure head

𝐾⏟ = intrinsic permeability tensor of element

𝑧 = datum 𝑑𝑆 = surface area of element

𝑑𝑉 = volume of element 𝜃= moisture content

𝐶𝑚= current moisture concentration

𝐶𝑚𝑚𝑎𝑥= maximum moisture concentration

𝐽⏟𝑑

= diffusion flux

𝐷⏟ = diffusion/dispersion tensor

𝑎𝑚= diffusion coefficient

𝜏 = Tortuosity

𝛿𝑖𝑗= Kronecker delta

𝑁𝑖, 𝑁𝑗 = shape functions

𝜃= moisture content

𝜌0𝑚 = undamaged mastic density

𝐾𝑑 = mastic desorption coefficient

𝑑𝑆 = surface area of element

𝑑𝑉 = volume of element

𝐶𝑗𝑑= dissolved mastic concentration at node (j)

𝐷⏟𝑚

= diffusion tensor

∅ = porosity

𝛼 = compressibility coefficient of the material

ℎ = head pressure

𝑛⏟ = outward unit normal

TSR = tensile strength ratio

IDTw = average indirect tensile strength for the conditioned set

IDTD = average indirect tensile strength for the unconditioned set

ΓTotal = Total SFE

ΓLW = nonpolar component

ΓAB = acid-base component

Γ+ = Lewis acid component

Γ- = Lewis base component

ΓmLW, Γm

− and Γm+ = SFE components of solid substrate material (asphalt binder or aggregate)

ΓLTotal, ΓL

LW, ΓL+ and ΓL

−= SFE total and components of liquid solvent

Γ𝑏LW, Γ𝑏

− and Γ𝑏+ = SFE components of asphalt binder

ΓaLW, Γa

− and Γa+ = SFE components of aggregate

Θ = contact angle

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LIST OF ABBREVIATIONS

SFE: Surface Free Energy

APA: Asphalt Pavement Analyzer

DWPM: Dynamic Wilhelmy Plate Method

MDR: Moisture Damage Ratio

ETG: Expert Task Group

FHWA: Federal Highway Administration

CT: Computed Tomography

RoAM: Raveling of Asphalt Mixes

BT: Blister Test

DAT: Direct Adhesion Test

NMAS: Nominal Maximum Aggregate Size

RAP: Recycled Asphalt Pavement

LAS: Liquid Anti-strip

HL: Hydrated Lime

SBS: Styrene Butadiene Styrene

PPA: Polyphosphoric Acid

DMA: Dynamic Mechanical Analyzer

DSR: Dynamic Shear Rheometer

IDT: Indirect Tensile

TSR: Tensile Stress Ratio

CM: Coarse Material

FM: Fine Material

PG: Performance Grade

AV: Air Voids

VMA: Voids in Mineral Aggregate

MD: Moisture Damage

AC: Asphalt Concrete

FT: Freezing and Thawing

DOT: Department of Transportation

IDTW: Average Indirect Tensile Strength for the conditioned set

IDTD: Average Indirect Tensile Strength for the unconditioned set

MEPDG: Mechanistic Empirical Pavement Design Guide

NCHRP: National Cooperative Highway Research Program

UIUC: University of Illinois at Urbana-Champaign

BBS: Bitumen Bond Strength

IFE: Interfacial Fracture Energy

PATTI: Pneumatic Adhesion Tensile Tester

JMF: Job Mix Formula

Pmax = Peak load from adhesion test (N)

E = Bond energy (J/m2)

ICT = Illinois Center for Transportation

COV = Coefficient of variance (%)

E* Ratio = dynamic modulus ratio

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CHAPTER 1 INTRODUCTION AND OVERVIEW

1.1 BACKGROUND

Moisture is one of the major sources of deterioration in flexible pavements. The

aggregate-binder interface has been studied in the presence of water since 1932 (Caro et al.

2008a). Moisture damage, defined as the degradation of the mechanical properties of asphalt

concrete caused by moisture (Zollinger 2005), was first recognized as a serious problem in the

early 1960s (Sebaaly et al. 2003). However, it was not until the 1980s that moisture damage

gained the attention of highway agencies and the pavement industry (Caro et al. 2008a).

Mogawer et al. 2002 reported in a study surveying 27 states that 15 suffered moisture-related

problems.

Despite the improvements and developments of asphalt mixture design procedures and the better

understanding of the mechanisms of moisture damage, it is still considered one of the most

common and complex problems facing the pavement community (Wasiuddin et al. 2007a,

Wasiuddin et al. 2007b). Moisture damage causes a severe loss in the strength and durability of

asphalt pavements, leading to a major decrease in pavement performance. It also contributes

significantly to the premature deterioration of asphalt pavement, which results in an additional

$54 billion annual vehicle operating costs (Caro et al. 2008a).

Generally, the existence of moisture in asphalt pavements separates the asphalt film from

aggregate particles, thus causing what pavement engineers call stripping. Stripping contributes to

several distresses, including thermal and fatigue cracking, rutting, and raveling cracking (Sebaaly

et al. 2003; Cho et al. 2009; Leatherman 2012; Huang et al. 2010; Tseng and Lin 2013). Error!

Reference source not found. shows different distresses caused by moisture damage captured in

winter 2013/2014 in Urbana-Champaign, IL. Moisture damage leads to and significantly

accelerates the previously mentioned distresses (Sebaaly et al. 2003).

It should be noted that moisture impact on Portland concrete pavements is different than that on

asphalt concrete. The impact on concrete pavements manifested in wrapping and curling of

concrete slab (Mukhopadhyay et al. 2006). This lead to the formation of cracks and/or the

separation between pavement structure layers. Moisture also penetrates into concrete pavement

structure through cracks and failing joints in jointed concrete pavements (Wang and Zollinger,

2000). The moisture presence may result in distresses such as pumping, spalling, faulting, and D-

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cracking (Mukhopadhyay et al. 2006). In the case of asphalt pavement, different distresses are

triggered by moisture such as rutting, fatigue cracking, raveling and bleeding. The distresses in

asphalt pavement are due to the impact of moisture on asphalt mix (causing debonding between

aggregate and binder) and/or pavement structure. Laboratory freezing and thawing cycles on

Portland concrete is usually conducted following AASHTO T 161 while for asphalt concrete it is

AASHTO T 283. In AASHTO T 161, the concrete samples are subjected to at least 300 freezing

and thawing cycles which can be increased to 500 if rigorous testing is required. In case of AC,

the number of freezing and thawing cycles is significantly less. In fact, the AASHTO T 283

requires one freeze and thaw cycle and the agencies could increase the number of freezing and

thawing cycles to reflect the severity of local environmental conditions.

Asphalt pavement permeability has a major impact on its durability and, hence, the degree of

damage induced by moisture (Torres 2004; Masad et al. 2006c; Tarefder and Ahmad 2015;

Bhattacharjee and Mallick 2002). Asphalt pavement permeability control could reduce moisture

damage. Mercado 2007 reported that moisture penetrates into pavement via three ways, namely

infiltration, evaporation, and capillary rise. The permeability increases with the propagation of

cracks in asphalt pavement. Tarefder and Ahmad 2015 reported that very few studies focused on

the relationship between the permeability of asphalt pavement and moisture damage. It was

reported that permeability has an exponential relation with air void content (Chen et al. 2004;

Tarefder and Ahmad 2015).

The permeability varies based on asphalt mix type (stone mastic asphalt, open-graded, or dense-

graded). Typically open-graded AC is designed with interconnected air voids (i.e. high

permeability) to drain the moisture away from asphalt pavement. Stone mastic asphalt has also

high permeability due to its aggregate skeleton structure; but less than open-graded. Dense

graded AC mixes have less interconnected air voids and so the least permeability amongst AC

mixes.

Generally, as air void content increases, the asphalt pavement strength decreases. Therefore,

open-graded AC mixes has the least strength amongst the aforementioned AC mixes (Chen et al.

2004). Chen et al. 2004 focused on dense-graded AC mixes and found that mixes with high air

voids (high permeability) refer to poor compaction and considered to be more moisture

susceptible. Similar results have been reported by Tarefder and Ahmad 2015. In addition,

Tarefder and Ahmad 2015 reported that, pavement structures in which the top layer had low

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permeability or higher permeability with respect to bottom layers showed a better field

performance compared to pavement structures that have all layers with high permeability.

Studying moisture damage is considered complex because of the diversity of resulted failure

mechanisms and the multiple study approaches. The failure mechanisms of moisture damage are

categorized into three main types (Cheng et al. 2003; Terrel et al. 1994):

1. Loss of cohesion and stiffness in asphalt mastic.

2. Loss of adhesion between the asphalt mastic and aggregates.

3. Degradation or fracture of aggregates because of freezing and thawing cycles.

The approaches for studying moisture damage include the following:

1. Evaluating traditional additives and modifiers used to mitigate moisture damage.

2. Evaluating and studying different aspects and causes of moisture damage.

3. Evaluating conventional moisture damage tests and comparing or correlating them with

field results.

4. Studying and evaluating new additives and modifiers.

5. Developing new tests, parameters, and analytical methods to improve moisture resistance

and moisture susceptibility predictions and measurements.

Many additives are used to mitigate the effect of moisture on asphalt concrete, and new types of

additives are being produced, studied, and evaluated. Hydrated lime and liquid anti-strip

additives are traditional additives that are widely used in the United States.

The moisture sensitivity of asphalt concrete depends on many factors, including aggregates and

binders properties, asphalt mixture properties, environmental conditions (e.g., temperature and

humidity), traffic loading, quality of construction, and pavement design (Sebaaly et al. 2007a;

Bhasin et al. 2007a; Hao et al. 2006; Leatherman 2012; Hicks 1991; Tseng and Lin 2013;

Zaniewski and Viswanathan 2006).

Moisture susceptibility or sensitivity has been studied in the lab using several conventional test

methods. The conventional tests are applied on loose and compacted samples. Most tests applied

on compacted samples, such as Lottman test (AASHTO T283), measure the mechanical

properties of the asphalt mixture before conditioning (dry sample) and after conditioning (wet

sample). A ratio threshold introduced between these two measurements (wet and dry) is used; the

minimum accepted value for this ratio differs from state to state. Other tests measure indices

including index obtained from Hamburg wheel tracking test measurement (Peiwen et al. 2006).

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These conventional tests indicate asphalt concrete sensitivity to moisture, yet they are considered

empirical tests and do not correlate very well with the moisture sensitivity of pavements in the

field due to the limitations in simulating field conditions in the lab (Kim et al. 2008).

In order to overcome the deficiencies of conventional tests, new tests such as the Moisture

Induced Sensitivity Tester (MIST) was introduced. The MIST device was developed recently in

an effort to better simulating field conditions (InstroTek 2012; Htet 2015). MIST mainly

simulates the pore pressure occurring in the field due to traffic loading. Samples in MIST are

conditioned under stress, water and high temperatures to accelerate potential moisture damage.

In order for an AC mix to be moisture resistance, it has to meet the requirements of at least two

of three criteria: density (swelling) and indirect tensile strength before and after conditioning and

visual inspection. Liang 2008 compared MIST to AASHTO T283 and found that the AASHTO

T283 is time consuming, results depends on degree of saturation and incapable of simulating

pore pressure.

In addition, other concepts are being used, such as surface free energy (adhesion and cohesion

energies), diffusion, and fracture parameters (Kim et al. 2008). Modeling has also been used to

help better understand moisture damage and to predict pre-construction pavement performance

in the field.

1.2 MECHANISMS OF MOISTURE DAMAGE

When moisture or water exists in asphalt concrete, it creates damage, and this damage is

governed by a mechanism that consists of two stages (Caro et al. 2008a):

1. Transport of moisture (vapor or liquid) through asphalt concrete, asphalt binder, or

mastic.

2. Degradation of the mechanical properties of asphalt concrete and loss of its strength

capacity because of moisture.

Both stages are subject to the characteristics of asphalt and binder, asphalt mixture,

environmental conditions, and traffic loading. In general, the above responses can be categorized

into three main types of moisture damage mechanisms (Cheng et al. 2003; Terrel et al. 1994;

Leatherman 2012):

1. Stripping: loss of adhesion.

2. Softening: loss of cohesion.

3. Aggregate degradation.

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1.2.1 Asphalt Mixture Stripping

Stripping is defined as the physical separation of asphalt binder or mastic from the

aggregate as a result of the loss of adhesion caused by moisture (Caro et al. 2008a). The adhesion

between the aggregate and asphalt binder or mastic depends primarily on seven factors (Terrel et

al. 1994):

1. Binder viscosity.

2. Chemical composition of binder and aggregate.

3. Surface energy components of binder and aggregate.

4. Cleanliness of aggregate.

5. Amount of mixture in aggregate and mixing temperature.

6. Aggregate porosity.

7. Aggregate texture.

1.2.2 Binder Softening

Softening is a reduction in stability and strength caused by the loss of cohesion in asphalt

binder because of moisture (Wasiuddin et al. 2007a; Wasiuddin et al. 2007b). Moisture affects

cohesion of asphalt binder through intrusion, saturation, or swelling. Cohesion depends primarily

on binder viscosity (Terrel et al. 1994).

1.2.3 Aggregate Degradation

The aggregate is fractured during degradation. This occurs especially when the asphalt

mixture is subjected to freezing and thawing cycles (Cheng et al. 2003).

The aforementioned three mechanisms take place in different forms because moisture transports

into the asphalt mixtures through different modes. The forms of the mechanisms of moisture

damage include (Caro et al. 2008a):

1. Detachment: Separation of aggregate and mastic at the interface because of the existence

of a thin film of water. This form is related to the stripping mechanism.

2. Displacement: In this response, the aggregate degrades as a result of breaking in the

asphalt film and/or weakening of aggregate-binder bond at the interface. This form can be

related to the loss of adhesion and/or to aggregate degradation mechanisms.

3. Dispersion of mastic: The cohesive bond in the mastic weakens as a result of long-term

diffusion periods. This form is related to the softening mechanism.

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4. Desorption of mastic: The outer layers of the mastic are washed away because of the

high-speed flow of moisture. Desorption is related to the softening mechanism.

5. Spontaneous emulsification: This form is also related to the softening mechanism, where

droplets of water are emulsified inside the mastic.

6. Film rupture or microcracks: In this form, deterioration and microcracks occur in the

aggregate or mastic. The microcracks generally reduce the strength of the asphalt

concrete system and simultaneously open new paths for moisture to move through. This

form can be attributed to the cohesion and aggregate degradation mechanisms.

1.3 LABORATORY EVALUATION OF MOISTURE DAMAGE

Moisture damage has attracted attention throughout the United States as most

transportation agencies are studying this phenomenon for the purpose of implementing measures

to mitigate its severity. Most studies conducted by transportation agencies concentrate on two

main aspects: 1) finding the right additives to be added to asphalt mixtures to mitigate moisture

damage and 2) introducing methodologies and tests to specify, indicate, and measure moisture

susceptibility of asphalt concrete (Caro et al. 2008a). These tests are necessary for predicting the

amount of damage that asphalt concrete is expected to incur because of moisture and developing

standards to distinguish between acceptable and unacceptable moisture-resistant materials and

mixtures (Caro et al. 2008b).

1.3.1 Development of Moisture Damage Tests

Pavement engineers concentrated their efforts on the development of tests to evaluate and

capture moisture damage, sensitivity, or susceptibility and, at the same time, to study and

evaluate the effect of different additives on moisture sensitivity. This approach was first

considered at the beginning of the 20th century and is still being sought. Tarefder et al. (2009)

conducted an extensive search of evaluation tests and presented the following historical chain

development: boil test (1930s, 1980s), absorption effects (1940s), sonic test (1950s), immersion

compression (1950s), aggregate characteristics (1950s), water pressure pore size effect (1950s),

thermally induced pore pressure test (1960s), surface reaction test (1970s), pore pressure-double

punch (1970s), cyclic water pressure strength (1970s), desorption by solvent extraction (1970s),

inverse gas liquid chromatography (1980s), freeze-thaw pedestal (1980s), freeze-thaw

conditioning with strength test (1970s, 1980s), tracking device (1970s, 1990s), asphalt pavement

analyzer (1990s), pneumatic pull-off (1990s), net adsorption (1990s), environmental

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conditioning system (1990s), ultrasonic test (2000s), asphalt chemistry (2000s), cyclic

pressure/suction (2000s), modified Lottman test or indirect tensile ratio test (1990s, 2000s),

moisture-induced stress tester (2000s), AASHTO T-283 (2000s), Hamburg wheel track test

(2000s), environmental conditioning system, and simple performance test (dynamic modulus and

flow number) (2000s, ongoing).

Moisture damage undergoes physical, mechanical, chemical, and thermodynamic processes,

(Caro et al. 2008a); however, most of the tests above are based on comparing the mechanical

properties of asphalt mixtures before and after moisture conditioning (Bhasin et al. 2007a). But

this approach does not capture the real cause for moisture damage neither does it reflect the

effects of the components (binder and aggregate) and mixture properties on moisture damage

(Bhasin et al. 2007a). In addition, most of the aforementioned tests fail to simulate the field

conditions affecting asphalt concrete mixtures, such as environmental conditions, traffic, and

time (Terrel et al. 1994) and, therefore, the results are always poorly correlated with field

performance (Caro et al. 2008a, Caro et al. 2008b). Furthermore, the procedures followed by

most the above tests are empirical and their results depend on the moisture conditioning methods

(Caro et al. 2008a).

These drawbacks encouraged the development of a new set of tests that provided a more accurate

moisture sensitivity evaluation. The new tests investigate the components of asphalt mixtures

(binder and aggregate) by studying their properties and establishing relationships for the better

understanding and characterization of moisture damage (Caro et al. 2008a) and for determining

the ability of different additives and modifiers to mitigate moisture damage. It is noticed that the

test procedures used to measure the loss of strength and stiffness can also measure the cohesion

and adhesion caused by water effects (Terrel et al. 1994). The new tests include a conditioning

process that simulates the field and accelerates strength loss to obtain results that correlate with

field measurements (Terrel et al. 1994). Because of the new tests, new terminologies were

created, such as surface free energy (SFE), work of adhesion, work of cohesion, interfacial

conditions, diffusion, and other evaluation parameters. The new tests study and measure the

adhesive and cohesive properties, moisture’s mode of transport, and the identification and effect

of these measurements on moisture-susceptible mixtures.

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1.3.2 Classification of Moisture Damage Laboratory Tests

Moisture damage laboratory tests are classified based on several factors. Caro et al.

2008a followed a traditional classification based on the following factors:

1. Sample condition.

2. Sample conditioning process.

3. Loading type (static or dynamic).

4. Measured scale of performance (micro and macro scale).

Sample condition classification divides the aforementioned tests to three groups (Cho et al.

2007):

1. Tests applied on compacted samples such as Marshall stability test, Lottman test,

immersion wheel tracking test, and asphalt pavement analyzer (APA).

2. Tests applied on loose mixture samples such as water immersion method, electro-optic

colorimetry test, and net adsorption test.

3. Tests applied on the components of asphalt mixture (aggregate and binder) such as

dynamic Wilhelmy plate method (DWPM), drying and wetting (soaking) tests for

diffusion, and universal sorption device test.

Generally, the main difference between tests conducted on loose samples and those conducted on

compacted samples is that the first focus on the visual inspection of the status of aggregates

coated with binder before and after the samples are subjected to moisture, while the second

evaluate moisture damage by measuring a chosen mechanical property before and after the

samples are subjected to moisture. Tests applied on compacted samples have the ability to better

simulate and estimate moisture effect because they are performance-related parameters;

however, the contribution of asphalt binder properties, aggregate properties, and aggregate-

binder bond on moisture damage is not clear in these tests because these properties are

distributed in the sample and mixed with other mixture-related properties.

Whether the asphalt sample is loose or compacted, it should pass through a conditioning process,

which affects the outcomes of the applied test. The following are the most widely used

conditioning processes (Birgisson et al. 2007):

1. Boiling loose samples for a period of time.

2. Placing compacted samples in a water bath for a specific period of time.

3. Freezing and thawing cycles applied on compacted samples for a specific period of time.

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4. Vacuum saturating compacted samples, then loading them with stresses to simulate

traffic loads.

5. Vacuum saturating compacted samples, then applying pore pressure.

Caro et al. 2008a also developed a new classification system based on the main outcomes

obtained from the moisture damage tests used to evaluate moisture sensitivity of asphalt

mixtures. The outcomes could be either subjective qualification, quantification using a

performance index, or moisture damage ratio (MDR).

The subjective qualification factor includes tests that are based on visual or qualitative

assessment of moisture damage, such as boiling water test, static immersion test, and ultrasonic

method. Quantification tests are conducted on loose and compacted samples with and without

loading, such as net adsorption, pneumatic pull-off, and surface energy tests. Each test has its

unique performance parameter that is linked to moisture damage. These parameters are obtained

from chemical or mechanical tests. MDR tests simulate the deterioration resulting from moisture

in the field during a short period of time. This short period is achieved by using different

conditioning processes to accelerate damage, similar to those previously mentioned. The MDR is

based on finding a ratio between a measured parameter or multiple parameters under wet

condition (conditioned) to the same parameter or parameters measured in dry condition

(unconditioned). MDR tests are conducted using compacted asphalt samples; each MDR test has

its own identified threshold. These thresholds are developed based on simulation of lab

measurements or field measurements. Sometimes these thresholds are changed from one state to

another depending on observations and research studies. MDR values allow evaluating the

influence of several factors affecting moisture damage such as air void distribution or addition of

additives and modifiers. Examples of MDR tests are Lottman test, static creep test, and

environmental conditioning system with dynamic modulus or flow number.

1.3.3 Difficulties in Developing Moisture Damage Evaluation Tests

Federal Highway Administration (FHWA) Expert Task Group (ETG) prepared an

extensive state-of-the-art report on moisture damage, studying different aspects of moisture

damage, including the tests used to evaluate moisture damage. According to this report, it is very

difficult to develop a test that evaluates moisture damage accurately and simulates field

performance because of the following reasons:

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Properties of asphalt binder, temperature, and stresses change from point to point

according to vertical pavement thickness and horizontal plane.

Interactions between moisture damage and other failure mechanisms such as fatigue and

low temperature cracking. Fatigue and low temperature cracking affect the severity of

moisture damage because cracking serves as a new path for moisture.

Field performance simulation is very much related to ever changing factors such as

environmental conditions, traffic loading levels, and air void distribution.

The properties of the pavement mixture produced by the plant may not match the mix

design. This results in invalid and misleading lab predictions

Pavement properties depend on the construction season, which affects the level of

compaction and degree of initial densification under traffic.

Developing a new method to evaluate and characterize moisture damage is a challenging task.

The complexity is attributed to two main causes: first, moisture damage involves physical,

mechanical, and chemical processes; and second, moisture damage is dependent on variables that

are function of time such as binder properties. In summary, there is no general agreement on the

method that best evaluates moisture damage. Therefore, much work needs to be done to develop

a test or multiple tests that can accurately evaluate moisture damage and simulate field moisture

damage.

1.4 MODELING

Mathematical modeling is considered the most recent approach for evaluating and

understanding moisture damage (Caro et al. 2008a). The modeling of moisture damage has

become possible because of state-of-the-art computing tools and an understanding of the

chemical and physical processes of moisture damage; it helps predict the behavior of asphalt

concrete in the presence of moisture for any given environmental and traffic loading conditions

and the approximate timing of different failure patterns (Kringos et al. 2008a); it also allows for

a clear observation of how different properties of both components (aggregates and binder) and

mixture affect moisture damage (Caro et al. 2008b).

Two main aspects of moisture damage are modeled: modes of moisture transport and the

mechanism of failure modes. The main modes of moisture transport are (Caro et al. 2008a):

1. Permeability.

2. Suction.

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3. Vapor diffusion.

Moisture diffusion through mastic is the key, regardless of the mode of transport. Diffusion

causes two mechanism failure modes (Caro et al. 2008a; Kringos et al. 2008a): a) adhesion

failure, where moisture diffuses through the mastic toward the binder-aggregate interface, thus

weakening this bond; and b) cohesive failure, where moisture diffuses through the mastic film

only causing it to soften (Figure 1.2).

According to Kringos et al. (2008a), cohesive failure is caused by another physical process called

“washing away.” Washing away is the loss of mastic particles or loss of mastic concentration as

a result of fast water flow along with high water pressure gradient. Other nomenclatures for this

failure mode are “scouring” and “erosion” (Figure 1.3). The rate of washing away is somehow

related to mastic diffusion properties (Caro et al. 2008b).

Kringos et al. (2008a) introduced the “pumping action” which is another mechanism of failure.

This failure mode appears in the condition of traffic loading applied over saturated air voids. The

passing load forms a high pore pressure on the surrounding aggregates, thus causing additional

damage. This mechanism mode is considered a mechanical process because it is directly related

to the applied load (Figure 1.4).

The X-ray computed tomography (CT) technology, along with imaging analysis-related

techniques, assisted in modeling different modes of moisture transport (Figure 1.5).

Permeability, or moisture flow, was modeled using finite difference techniques and the Lattice

Boltzmann approach (Caro et al. 2008b). Both approaches determine the flow speed and pore

pressure at any point along the void structure of asphalt concrete. Based on these modeling

approaches (Caro et al. 2008b), horizontal permeability is approximately twice as great as

vertical permeability and is clear in regions with connected air voids; regions with low

concentration of air voids act as “bottleneck” for vertical permeability; and there is a significant

change in pore pressure and flow speed along the depth of asphalt concrete. These findings are

attributed to the heterogeneity and non-uniform distribution of air voids inside asphalt concrete.

Kringos et al. (2008a) also performed a modeling for moisture flow, diffusion, and erosion

processes. The following relations were established:

a. Moisture flow:

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12

∑ (∫ 𝑁𝑖𝐿(ℎ)𝑁𝑗𝑑𝑉

𝑉

)

𝑛

𝑗=1

𝑑ℎ𝑗

𝑑𝑡 + ∑ (∫ ∇𝑁𝑖 𝐾⏟ ∇𝑁𝑗𝑑𝑉

𝑉

) =

𝑛

𝑗=1

∫ 𝑁𝑖𝑆

𝐾⏟ (∇ℎ + ∇𝑧)𝑑𝑆 − ∫ ∇𝑁𝑖𝑉

𝐾⏟ ∇𝑧𝑑𝑉

(1)

where:

𝑁𝑖, 𝑁𝑗 = shape functions

𝐿 = storage coefficient

ℎ = pressure head

𝐾⏟ = intrinsic permeability tensor of element

𝑧 = datum

𝑑𝑆 = surface area of element

𝑑𝑉 = volume of element

Equation 1 can also be written in the following matrix form:

[𝑚] {𝑑ℎ

𝑑𝑡} + [𝑆]{ℎ} = {𝐵} + {𝐺} (2)

b. Diffusion:

𝜃 = 𝐶𝑚

𝐶𝑚𝑚𝑎𝑥 (3)

𝐽⏟𝑑

= − 𝐷⏟ ∇𝐶𝑚 (4)

𝐷⏟ = 𝑎𝑚𝜏𝛿𝑖𝑗 (5)

where:

𝜃= moisture content

𝐶𝑚= current moisture concentration

𝐶𝑚𝑚𝑎𝑥= maximum moisture concentration

𝐽⏟𝑑

= diffusion flux

𝐷⏟ = diffusion/dispersion tensor

𝑎𝑚= diffusion coefficient

𝜏 = tortuosity

𝛿𝑖𝑗= Kronecker delta

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13

The amount of moisture mass in mastic at time (t) is dependent on the diffusivity which is

represented by the diffusion coefficient and the maximum moisture concentration.

c. Washing away:

∑ (∫ 𝑁𝑖(𝜃 + 𝜌0𝑚𝐾𝑑)𝑁𝑗𝑑𝑉

𝑉

)

𝑛

𝑗=1

𝑑𝐶𝑗𝑑

𝑑𝑡 + ∑ (∫ (∇𝑁𝑖 𝐷⏟ ∇𝑁𝑗) 𝑑𝑉

𝑉

) 𝐶𝑗𝑑

𝑛

𝑗=1

+ ∑ (∫ 𝑁𝑖𝛼 ∗𝜕ℎℎ

𝜕𝑡(𝜃 + 𝜌0

𝑚𝐾𝑑)𝑁𝑗𝑑𝑉

𝑉

)

𝑛

𝑗=1

𝐶𝑗𝑑 − ∑ (∫ 𝑁𝑖 (𝛼 ∗

𝜃

𝜕ℎℎ

𝜕𝑡) 𝑁𝑗𝑑𝑉

𝑉

)

𝑛

𝑗=1

𝐶𝑗𝑑

= ∫ 𝑁𝑖

𝑆

𝑛⏟ 𝐷⏟𝑚

∇𝐶𝑑𝑑𝑆

(6)

where:

𝑁𝑖, 𝑁𝑗 = shape functions

𝜃= moisture content

𝜌0𝑚 = undamaged mastic density

𝐾𝑑 = mastic desorption coefficient

𝑑𝑆 = surface area of element

𝑑𝑉 = volume of element

𝐶𝑗𝑑= dissolved mastic concentration at node (j)

𝐷⏟𝑚

= diffusion tensor

∅ = porosity

𝛼 = compressibility coefficient of the material

ℎ = head pressure

𝑛⏟ = outward unit normal

Equation 6 can also be written in a matrix form as follows:

[𝑚] {𝑑𝐶𝑑

𝑑𝑡} + ([𝐷] + [𝐾]){𝐶𝑑} = {𝑄} + {𝐵} (7)

Equations 1 through 7 are applied on the mesh shown in Figure 1.6.

This micro-scale finite element model was used to simulate moisture-induced damage because of

the different processes mentioned above. The simulation model consists of two particles of

aggregates coated with mastic and has fully saturated pores which were simulated as porous

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14

media formulation. To simulate the diffusion effect on the bond, the aggregate-mastic interface

was also modeled.

To determine whether the moisture-induced damage is in mastic or at the aggregate-mastic bond

interface, it is necessary to measure the moisture diffusion coefficient of mastic (Kringos et al.

2008a). A coefficient of mastic sorption test was conducted to determine moisture diffusion. In

this test, a small sample of mastic was placed in a chamber and subjected to moisture vapor. The

weight of the mastic sample was known and recorded before and during the test. The difference

in weight is caused by the moisture diffusing through the mastic sample. The diffusion

coefficient of mastic was therefore determined.

Kringos et al. (2008a, 2008b) developed a finite element routine called raveling of asphalt mixes

(RoAM) at the Delft University of Technology, the Netherlands. The RoAM routine is part of

the CAPA-3D finite element software. Equations 1 through 7 are embedded in this routine,

which reflects a numerical simulation of diffusion that results in adhesive, cohesive, and washing

away failures. This routine also simulates the pumping action failure mode. The most interesting

feature of this routine is that it exclusively models and analyzes moisture damage.

The modeling of moisture needs further study, analysis, and development. Other factors can be

introduced in the future modeling process such as simulating the effect of additives on asphalt

mixtures, adding more components and mixture properties related to moisture damage, and

considering additional environmental and traffic loading conditions.

1.5 PROBLEM STATEMENT

Many laboratory tests have been developed to understand and evaluate moisture damage.

Laboratory tests are conducted on asphalt concrete mixture and component (binder and

aggregate) levels using various conditioning procedures to introduce the effects of moisture.

Mixture-level tests usually evaluate moisture damage based on two concepts: visual observation

of the moisture effect and comparison of a specific mechanical property before and after

introducing the moisture effect, which is a more common concept. This comparison results in a

ratio or an index used to identify the asphalt concrete potential moisture susceptibility.

Current mixture laboratory tests have three main drawbacks: limited ability of simulating

environmental conditions, dependence of results on the test conditioning process, and limited

correlation between laboratory and field results. These shortcomings have compelled the

development of new tools to study moisture damage especially at the component level. The SFE,

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15

blister test (BT), and direct adhesion test (DAT) are examples of component-level tools

introduced to study the compatibility between aggregate and binder in the presence of moisture.

1.6 OBJECTIVE AND SCOPE

The main objective of this study is to predict moisture susceptibility of asphalt concrete

from component-level testing. To achieve this objective, various conditioning and aging levels

are considered for both mixture and component testing levels.

The study focused primarily on the study of the effects of moisture on asphalt mixtures. Two

asphalt mixes (in addition to selected additives and modifiers), typically used in the State of

Illinois, were considered: 19.0mm nominal maximum aggregate size (NMAS) binder mix and

19.0-mm NMAS mix with 50% recycled asphalt pavement (RAP). The additives and modifiers

consist of liquid anti-strip (LAS), hydrated lime (HL), styrene butadiene styrene (SBS), SBS

with LAS, and polyphosphoric acid (PPA) with HL.

The combinations of additives and modifiers were used with the 19.0-mm NMAS mix. No

additives or modifiers were used with the 50% RAP mix. The effects of the additives and

modifiers on the moisture susceptibility of the proposed asphalt mixtures were evaluated through

several mixture- and component-level tests. The mixture-level tests are the modified AASHTO

T-283 and dynamic modulus tests. The surface free energy (SFE), direct adhesion test (DAT),

and blister test (BT) represent the component-level types.

The study also addressed with the possible long-term effects of additives and modifiers on the

moisture resistance of asphalt mixes. Samples for the mixture-level tests were prepared at

different aging and conditioning durations. Aging durations include one hour and four hours after

mixing and prior to compaction; conditioning durations comprise one thawing cycle, three

freezing and thawing (FT) cycles, and five FT cycles. Aging was also being considered at the

component level by using the rolling thin film oven (RTFO) and pressure aging vessel (PAV).

Each binder was tested at the virgin, RTFO, and PAV aging status.

The impact of this study can be summarized in the following bullets:

1. Evaluate the impact of additives/modifiers, short-term aging, and conditioning on the

moisture susceptibility of asphalt mixes.

2. Evaluate the moisture susceptibility of asphalt mixes using the dynamic modulus test.

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3. Based on the latest knowledge of the author this is the first study to evaluate the impact

of additives/modifiers (especially HL) along with aging (short-term and long-term) using

Sessile drop device, BT and DAT.

4. Based on the latest knowledge of the author this is the first study to evaluate the impact

of RAP at the component level.

5. This study is one of few to verify the ability of Sessile drop device to measure the SFE of

aggregate.

1.7 THESIS ORGANIZATION

This thesis focuses on understanding moisture damage in asphalt mixtures specifically by

evaluating moisture susceptibility using component-level tests. The thesis is divided into seven

chapters. In addition to the problem statement, objectives and scope of the study, Chapter

1 includes a literature review discussing moisture damage mechanisms, evaluation techniques

and modeling. Chapter 2 discusses the materials (aggregate, asphalt binder, and

additives/modifiers) and asphalt mix used in this study. Chapters 3 and 4 focus on the mixture-

level and component-level tests conducted to evaluate asphalt mix moisture susceptibility.

Chapter 5 and Chapter 6 reports the outcomes obtained from the mixture- and component-level

tests respectively along with a detailed discussion of the test results Chapter 7 discusses the

relationship between the results obtained from the mixture and component-level tests. Finally,

Chapter 8 summarizes the major findings and conclusion and makes suggestions and

recommendations for future research.

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17

(a) (b)

(c) (d)

(e)

(f)

Figure 1.1 Fatigue cracking, rutting, raveling and potholes captured in winter 2013/2014 in

Urbana-Champaign, IL.

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18

(g)

(h)

(i)

(j)

(k)

(l)

Figure 1.1 (continued)

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19

(m)

(n)

(o)

(p)

(q)

(r)

Figure 1.1 (continued)

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20

(s)

(t)

Figure 1.1 (continued)

(a) (b)

Figure 1.2 Effect of moisture diffusion: (a) cohesive failure and (b) adhesive failure

(Kringos et al. 2008a).

Figure 1.3 Mastic erosion caused by fast flowing water (Kringos et al. 2008a).

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21

Figure 1.4 Pumping action mechanism (Kringos et al. 2008a).

Figure 1.5 3D X-ray CT with imaging analysis technique (Kassem et al. 2006).

Figure 1.6 Finite element mesh for modeling moisture damage (Kringos et al. 2008b).

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22

CHAPTER 2 MATERIALS AND ASPHALT MIX

2.1 MATERIALS

A binder mix from District 5 of the Illinois Department of Transportation (IDOT) was

chosen for this study. The mix is designated as N90; number 90 represent the design number of

gyrations. This mix was chosen because it is moisture susceptible, as indicated by tensile

strength ratio (TSR) results.

2.1.1 Aggregate

N90 mix uses three aggregate stockpiles—two coarse (CM11 and CM16) and one fine

(FM20). CM11, CM16, and FM20 were imported from a quarry in Kankakee, IL., and are

considered to be dolomitic limestone.

The current state of knowledge in the literature suggests that dolomitic limestone generally

produces AC that is relatively unsusceptible to stripping. However, this was not the case. In

addition to these aggregate stockpiles, mineral filler imported from Thornton, IL., was used.

Table 2.1 presents the aggregate gradations and physical properties.

Despite the fact that only one aggregate type (believed to be susceptible to moisture damage) is

used in this study, it should be noted that the aggregate type plays a major role in the degree of

moisture susceptibility of AC mixture. Apeagyei et al. 2015 studied the physico-chemical

properties of aggregate and its relation to moisture damage and found that generally the higher

the aggregate moisture absorption the higher the moisture susceptibility. Airey et al., 2007

showed that aggregates’ mineralogical and chemical composition had more impact on moisture-

induced damage severity in comparison to binder properties.

2.1.2 Asphalt Binder

The base asphalt binder used in N90 mix was the unmodified PG 64-22. The asphalt

binder was obtained from Heritage Laboratories, Inc.

2.1.3 Additives/Modifiers

Asphalt binder may be modified in one or more of the following three processes (Bhasin

and Little 2009):

Performance grade (PG) modification: In this form, polymers are generally added to

binder to increase its PG; especially for high service temperature or high traffic levels.

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This modification is in accordance with the Superpave® specifications. The original

binder (before modification) is called base binder.

Mixture performance modification: Enhancing asphalt mixture performance by adding

special material to binder such as liquid antistripping (LAS) agent. The main goal of

adding the LAS is to increase moisture resistance of the asphalt mixture. Materials can be

added to base binders or to binders that are already modified.

Environmental modification (e.g., asphalt concrete aging): Aging leads to changes in the

chemistry and mechanical properties of asphalt binder.

Additives and modifiers are considered two of the most cost-effective measures used to mitigate

moisture damage (Zaniewski and Viswanathan 2006). Performance grade and mixture

performance modifications generally increase the bond energy between the binder and aggregate

by decreasing the surface tension of binder (Expert Task Group 1990). Additives, such as

hydrated lime (HL), can be added to binder or aggregate.

When designing an asphalt mixture and an additive or a modifier needs to be chosen to reduce

the moisture damage affect, the following should be taken into consideration (Expert Task Group

1990):

1. Dosage: amount to be added to the mix.

2. Economics: availability and cost effectiveness.

3. Effect of this modification on adhesive and other mixture properties.

Many additives are developed throughout the United States to be added to asphalt mixtures. The

primary aim of using additives is to reduce moisture sensitivity and stripping. These additives

can be found naturally or are chemically processed. LAS and HL are two common additives used

in the United States to increase moisture resistance. Despite their benefits, LAS and HL may

result in the need for early pavement maintenance and rehabilitation, thus increasing economic

costs (Tunnicliff and Root 1984), if used incorrectly or added when not needed.

In addition to LAS and HL, two polymers were considered in this study, namely SBS and

Polyphosphoric Acid (PPA). LAS, HL, SBS and PPA were used in this study because they are

the most widely used additives and modifiers in Illinois asphalt mixes.

2.1.3.1 Hydrated Lime

Lime additive has been used in asphalt mixtures since 1910. Lime is thought to control

stripping by increasing the adhesion energy between the aggregate and binder through decreasing

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24

the interfacial tension between the binder and water. This stripping resistance can be chemically

described as the lime reacting with the carboxylic acids in binder, forming insoluble compounds

that are absorbed onto the aggregate surface. Lime is added to asphalt mixtures by any of the

four following methods:

1. Dry lime to dry aggregate: In this method, dry lime is first added to the aggregate and

then the binder is added to the mixture. However, a significant amount of lime is lost

from the surface of aggregate during the drying process; especially in the drum before the

binder is added.

2. HL slurry: The lime is added to aggregate and then marinated by adding water to this

composition. After marinating, the aggregate enters the heating process and the binder is

added. However, an additional cost of fuel is incurred in this method for extracting the

additional amount of water added to the marinating process.

3. Dry HL with moist aggregate: This method differs from the HL slurry method in that the

aggregate water content is increased by 3% to 5%, and then lime is added to this moist

aggregate for marinating. This composition then enters the plant for heating and the

binder is added for mixing.

4. Hot slurry: In this method, the lime is heated before it is added to the aggregate. Then

water is added, followed by the binder. This method is considered very hazardous and

affects the safety of plants workers because of the high temperature that results from

adding water to the hot lime and aggregate.

Lime dosage ranges between 0.5% and 2% by the weight of aggregate (Expert Task Group

1990). Adding lime to asphalt mixtures increases its cost by approximately $2 to $4 per ton

(Expert Task Group 1990). The overall performance of asphalt mixture with lime is acceptable in

the field and lab when studying rutting, resilient modulus, tensile strength and TSR (Birdsall

1999; Kennedy and Anagnos 1984; Mohammad et al 2000). However, the effectiveness of lime,

when used with other additives, depends on the type of aggregate and binder used in the mix.

Lime is not effective when added to specific types of aggregates. The method used to add lime to

the asphalt mixture also affects overall performance (Expert Task Group 1990).

In general, the improvement of AC stiffness, increase in rutting and cracking resistance, and

reduction in oxidation and aging over time are the three major benefits of adding lime to AC

(Hicks and Scholz 2001; Khosla and Harikrishnan 2007; Lesueur and Little 1999; Little and

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25

Epps 2011; Mohammad et al. 2000; Petersen et al. 1987). In this study, the lime used was

imported from Mississippi Lime Company. This lime is considered high in calcium content.

2.1.3.2 Liquid Anti-strip

There are many types of LAS additives, but most of them are considered surface-active

agents. The selection of LAS type and amount should be based on mix characteristics and

conditions. When added to AC mixture, LAS contributes to the reduction of the surface tension

of asphalt binder and, consequently, to the increase of adhesion between the aggregate and

binder. In other words, adding LAS increases the wettability of aggregate, meaning that the

aggregate will be more easily wetted by asphalt binder. Other studies show that adding LAS to

asphalt binder results in enhancing the aging properties, reducing temperature susceptibility, and

softening (Anderson and Dukatz 1982; Khosla and Harikrishnan 2007). Anderson and Dukatz

1982 had shown that the impact of liquid antistrip is asphalt source dependent.

One of the main challenges of using LAS is heat degradation, which occurs when holding the

asphalt mix at high temperatures for a long period. Head degradation reduces LAS effectiveness

(Khosla and Harikrishnan, 2007; Tayebali, 2003; Zaniewski and Viswanathan 2006).

Generally, the dosage of LAS ranges between 0.1% and 3% by the weight of asphalt binder

(Expert Task Group 1990). The dosage of LAS differs from one mix to another because of the

different properties of binder and aggregate found in each mix. LAS is either added to the asphalt

binder before mixing it with the aggregate, or it is added to the aggregate before adding the

binder. Because LAS needs to be efficient and provide the user with the best benefits, most of

the added LAS should be at the interfacial region between the aggregate and binder. Therefore, it

is obvious that adding the LAS to the aggregate assures the presence of anti-strip at the interface

more than the first method. The immigration of LAS through the binder to reach the interface is

not easy and depends on the viscosity of the binder.

Many transportation agencies report a difference between the performance of asphalt mixtures

with LAS in the field and in the laboratory. This finding may be attributed to any of the

following (Expert Task Group 1990):

1. The LAS was not properly mixed with the binder.

2. The use of wet aggregate.

3. Improper dosage amount or improper type of LAS.

4. The moisture evaluation tests conducted in the laboratory are not representative enough.

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5. Lack of heat stability.

2.1.3.3 Styrene Butadiene Styrene

The use of binders modified with SBS polymer is one of the methods used to produce an

asphalt concrete mixture that is more stripping resistant. The chemical structure of SBS consists

of styrene (C6H5–CH=CH2)n, butadiene (CH2=CH–CH=CH2)n, and styrene (C6H5–

CH=CH2)n, where subscript (n) represents the number of repeating units in the polymer

molecule (Tarefder et al. 2009). When (n) is equal to 1, the polymer is called SBS monomer

polymer. The combination of many monomers forms a polymer. Polymer molecules can be

simply linearly chained where the monomers are aligned in one linear line, or cross-linked when

several linear chains bond together in three dimensions (Tarefder et al. 2009).

Regarding the setting characteristics, polymers are classified as thermosetting polymers and

thermoplastic polymers. SBS is considered one of the thermoplastic polymers; under high

temperatures, it softens and becomes workable and can be easily added and mixed with asphalt

binder. At room temperature, SBS has rubber-like properties, and when cooling, it hardens and

maintains its shape and loses the rubber properties (Tarefder et al. 2009). The only way to add

polymer to asphalt mixture is by adding it to a heated asphalt binder (190°C approximately) and

then mixing the modified binder for a period of two hours in a special mixer to assure proper and

homogenous distribution of the polymer (Tarefder et al. 2009).

2.1.3.4 Polyphosphoric Acid

Polyphosphoric acid (PPA) is a liquid mineral polymer that has many applications,

including asphalt modification which enhances asphalt concrete to resist moisture effects and

improves the high temperature performance grade as well as the low temperature performance

grade for a few asphalt binder types. PPA can be used exclusively or with other polymers such as

SBS or other additives such as lime or LAS. All three (PPA+modifier+additive) can also be used

together in asphalt mixtures, but with different PPA percentages for each.

The user of PPA must be careful with LAS additives because a neutralization reaction may occur

as a result of PPA reacting with some types of LAS; this means that the asphalt binder loses its

stiffness, but not its adhesion properties (Buncher 2010). Different results are observed with the

lime additive because PPA does react with lime. Additionally, PPA does not react efficiently

with limestone aggregates (Kutay et al. 2007a) while it is very efficient with acidic aggregate

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27

types such as granite (Buncher 2010). PPA is considered a relatively new additive and needs to

be further studied and evaluated to be used as a moisture damage controller.

Although this literature review covers four additives only, more additives are used in the United

States, including Portland cement, fly ash, and flue dust (Sebaaly et al. 2007a). As a rule of

thumb, the effectiveness of any additive depends on the type of binder and aggregate used in the

asphalt mixture.

The performance of the four additives mentioned above has never been compared; however, the

performance of lime and LAS (Lu et al. 2006; Peiwen et al. 2006; Sebaaly et al. 2007a) was

compared, and it was observed that both lime and LAS improve moisture resistance in short-term

aging. The moisture resistance of lime and LAS decreases in long-term aging, but the rate of

decrease for the LAS is greater than that for lime. It was concluded that using lime-treated

mixtures improves the moisture resistance on the short and long term aging (Huang et al. 2009;

Kim et al. 2008; Mohammad et al. 2008; Sebaaly et al. 2003), and that using lime increases the

pavement service life by an average of three years (Sebaaly et al. 2003). On the other hand, as

indicated earlier, LAS increases the adhesion energy between the binder and aggregate, thus

creating more moisture resistant mixtures (Wasiuddin et al. 2007a; Bhasin et al. 2007b, Bhasin

and Little 2009). If not used with proper binder and aggregate types, LAS will not affect

moisture susceptibility and, in some cases, may increase it (Bhasin and Little 2009). It was

observed that SBS additive increases moisture resistivity when added with unaged and aged

binder (Tarefder et al. 2009; Bhasin and Little 2009). In general, the long-term performance of

many additives is still unclear because of the lack of long-term performance data for some

additives (Expert Task Group 1990).

2.2 ASPHALT MIX

Before initiating laboratory tests, the mix design for N90 mix was verified. Accordingly,

buckets of aggregate were sampled from the stockpiles, dried, and sieved. Next, the gradation,

bulk specific gravity, absorption, and loose and rodded unit weights were determined for each

aggregate stockpile. The Bailey method was used to determine aggregate blend percentages and

asphalt binder content necessary to achieve the required mix volumetrics. The design mix

volumetrics for the N90 mix were 13.8% and 4.0% voids in the mineral aggregate (VMA) and

air voids (AV), respectively. After determining designs that provided the desired volumetrics

within ± 0.1%, the next step was to optimize the asphalt binder contents. Table 2.2 shows the

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final aggregate blend percentages and asphalt binder contents, along with the volumetrics for

N90 mix.

In addition to the N90 mix (control), five more mixes were prepared using the aforementioned

four various additives and modifiers. The five mixes are namely control +LAS, control+SBS,

control+SBS+LAS, control +HL and control+PPA+HL. The control, control+LAS,

control+SBS, control+SBS+LAS mixes had the same aggregate blend percentages and asphalt

binder content. In the case of mixes with hydrated lime (control +HL and control+PPA+HL),

aggregate and asphalt binder percentages were minimally adjusted to achieve the same

volumetrics (VMA and AV) as the control mix, as shown in Table 2.3.

Recycled asphalt pavement (RAP) was also used in this study as 50% RAP was added to the

control mix. The addition of 50% RAP changed the aggregate gradation and binder content, but

the 50% RAP mix had the same VMA as the control mix and, therefore, as the other mixes, see

Table 2.4, (Aurangzeb et al. 2012).

LAS, SBS, and PPA were added to asphalt binder. LAS was added in the lab, while SBS and

PPA were added by the asphalt binder supplier. The amount of SBS and PPA added to the

asphalt binder was sufficient to bump the PG from 64-22 to 70-22. The LAS content used was

0.75%. This LAS content was based on the results from the modified Lottman AASHTO T283-

02 test with five FT cycles on specimens with various LAS contents (1.0%, 0.75%, 0.50%, and

0.25%). The lime content adopted for the N90 mix was 1.0%, and was added to the aggregate.

The lime addition in this study was done through the dry technique according to IDOT

specifications.

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Chapter 2 Figures and Tables

Table 2.1 Main Features of Aggregates: (a) Gradations (b) Aggregate Physical Properties

(a)

Sieve Size Aggregate Stockpile

CM11 CM16 FM20 MF

1" 100.0 100.0 100.0 100.0

3/4" 82.1 100.0 100.0 100.0

1/2" 39.1 100.0 100.0 100.0

3/8" 19.0 97.3 100.0 100.0

No. 4 3.9 36.7 98.6 100.0

No. 8 2.7 6.8 74.6 100.0

No. 16 2.4 3.1 43.9 100.0

No. 30 2.2 2.3 24.6 100.0

No. 50 2.1 2.2 14.5 100.0

No. 100 2.1 2.1 9.7 95.0

No. 200 2.0 2.0 7.1 90.0

(b)

Type of Material CM11 CM16 FM20 MF

Bulk Specific Gravity 2.6 2.6 2.6 2.9

Absorption (%) 2.0 2.6 2.1 1.0

Loose Weight (Ave)-(kg/m^3) 1450.4 1435.1 1628.8 ----

Rodded Weight (Ave)-(kg/m^3) 1610.0 1574.3 1824.9 ----

Solid Unit Weight-(kg/m^3) 2632.0 2620.0 2635.0 ----

Voids at Loose UW (%) 44.9 45.2 38.2 ----

Voids at Rodded UW (%) 38.8 39.9 30.7 ----

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Table 2.2 N90 Control Mix Designs

N90 (Control)

Mix

CM11 (%) CM16 (%) FM20 (%) MF (%) AC (%) VMA (%) AV (%)

38.7 38.2 21.8 1.3 5.2 13.8 4.0

Table 2.3 Mix Design of All N90 Mixes

Mix CM11 (%) CM16 (%) FM20 (%) MF (%) AC (%) VMA (%) AV (%)

Control, Control+LAS, Control+SBS,

Control+SBS+LAS

38.7 38.2 21.8 1.3 5.2 13.8 4.0

Control+HL, Control+PPA+HL

38.5 38.0 21.7 0.8 5.2 13.8 4.0

Table 2.4 RAP Mix Design

Mix CM11 (%)

CM16 (%)

RAP +3/8 (%)

RAP -3/8 (%)

FM22 (%)

FM20 (%)

MF (%)

AC (%)

VMA (%)

AV (%)

50% RAP

25.7 9.6 35.0 15.0 9.66 4.8 0.2 3.1 13.8 4.0

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CHAPTER 3 MIXTURE-LEVEL CHARACTERIZATION

3.1 INTRODUCTION

To study moisture damage of asphalt concrete, it is important to develop a set of tests that

can be used to evaluate the extent of moisture damage on asphalt mixture and the effects of

various additives on the mixture’s moisture sensitivity. Moisture damage is a complex

phenomenon that encounters physical, mechanical, chemical, and thermodynamic processes.

Most of the early developed tests concentrate on the mechanical process. There are three

problems with this approach (Zaniewski and Viswanathan 2006). First, it does not capture the

real cause of moisture damage and the actual effects of the components and mixture properties

on this phenomenon. Second, it does not simulate the real field conditions acting on AC

mixtures, such as environmental conditions, traffic, and time; therefore, the results are poorly

correlated with field performance. Third, most of the currently used tests are empirical, in which

the results depend on the moisture conditioning methodology. To overcome these drawbacks, a

new set of tests was developed. The new tests concentrated on the AC components’ behaviors

and their relationship to moisture damage, in addition to studying the effect of various additives

and modifiers on those behaviors.

Whether the AC sample is loose or compacted, it should undergo a conditioning process, which

affects the outcomes of the applied test. The most widely used conditioning processes are

vacuum saturating compacted specimens; placing compacted specimens in a hot water bath, and

possibly applying freeze-thaw (FT) cycles on compacted samples.

The Expert Task Group (ETG) of the Federal Highway Administration (FHWA) (Expert Task

Group 1990) authored a comprehensive, state-of-the-art report that evaluated different aspects of

moisture damage and the tests that can be used to assess it. According to this report, it is very

difficult to develop a test that accurately evaluates moisture damage and also simulates field

performance, for two reasons. First, moisture damage involves physical, mechanical, and

chemical processes. Second, this type of damage is affected by time-dependent variables such as

binder properties.

This research study proposes two mixture-level tests and three component-level tests. The

mixture-level tests are modified indirect tensile strength (AASHTO T-283) and dynamic

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modulus tests. The surface free energy, direct adhesion, and blister tests represent the

component-level tests.

3.2 ILLINOIS MODIFIED LOTTMAN (AASHTO T-283) TEST

The AASHTO T-283 test was developed by Lottman at the University of Idaho in 1982

(Hunter and Ksaibati 2002; Khosla and Harikrishnan 2007). Then, the test was well described in

NCHRP project 192 and field tested in NCHRP 246 (Hunter and Ksaibati 2002). After applying

several modifications on the original Lottman test procedure, AASHTO accepted the test in 1985

under “modified Lottman test (AASHTO T-283)” (Hunter and Ksaibati 2002).

The use of tensile stress parameter was found to be more suitable for studying moisture damage

as mixes were found to be more sensitive to tensile stress loading compared with other loading

modes (Moreno-Navarro et al. 2014). Because of that, AASHTO T-283 is considered one of the

most common tests used to evaluate AC moisture resistance (Khosla and Harikrishnan 2007;

Leatherman 2012; Williams and Breakah 2010). AASHTO T-283 was even adopted by

Superpave in its mix design procedure to check for moisture damage possibility (Khosla and

Harikrishnan 2007; Zaniewski and Viswanathan 2006).

Despite the popularity of AASHTO T-283 test, it holds several shortcomings including the

following (Azari 2010; Kandhal and Rickards 2002; Kringos et al. 2009a; Leatherman 2012;

Roberts et al. 1996; Zaniewski and Viswanathan 2006):

1. Tensile strength ratio values do not correlate with field performance.

2. Producing conflicting results between 6.0 in (150 mm) diameter gyratory sample

compared with 4.0 in (100mm) diameter Marshall Sample. The gyratory sample produces

fewer variable results while the Marshall sample has better correlation with the field.

3. Results change significantly based on the duration and severity of saturation.

4. Simulating traffic loading with constant rate is not realistic as compared with cyclic

loading.

Several studies conducted thorough revisions of AASHTO T283 procedure. NCHRP Project 9-

13 is one of these major studies. NCHRP Project 9-13 developed conclusions but unfortunately

overridden by the AASHTO committee and replaced by restrictions on the saturation and

conditioning process. Despite these restrictions, it was still found that AASHTO T283 “is not a

reliable method for evaluating the field performance” of AC (Epps et al. 2000, Zaniewski and

Viswanathan 2006).

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To evaluate whether the selected N90 control mix is moisture susceptible, the Illinois modified

Lottman test was conducted. This test is a modified version of the Modified Lottman AASHTO

T283 test; IDOT modified the test procedure by altering the sample conditioning process by

excluding the single freeze–thaw cycle. IDOT found that conditioning with a 24 hr soak in the

140°F (60°C) bath alone is more rigorous than a single freeze–thaw cycle (i.e., it more

significantly affects results compared with unconditioned mixes) (Khosla and Harikrishnan,

2007).

Each mix requires six specimens. The dimension of each specimen is 5.91 in (150 mm) in

diameter and 3.75 ± 0.20 in (95 ± 5 mm) in thickness. The air void content of each specimen

should be 7.0% ± 0.5%. The six specimens are divided into two groups: unconditioned and

conditioned sets. The average air void content for each set should be approximately the same.

Before the unconditioned set of mixtures are tested for indirect tensile (IDT) strength, they are

placed in a 77 ± 1.8°F (25 ± 1°C) water bath for 2 hr ± 10 min with at least 1 in (25 mm) of

water covering the specimens’ surface. The conditioning process starts by saturating each

specimen 70% to 80% of its air voids under a vacuum of 10 to 26 in Hg partial pressure (13 to 67

kPa absolute pressure). Then, the conditioned set of specimens are placed in a 140 ± 1.8°F (60 ±

1°C) water bath for 24 ± 1 hr. Finally, the specimens are transferred to a 77 ± 1.8°F (25 ± 1°C)

water bath for 2 hr ± 10 min. The conditioned specimens are then tested for their IDT strength, as

shown in Figure 3.1.

The average IDT strength is calculated for the unconditioned and conditioned sets in order to

calculate the TSR parameter. The TSR is the ratio of the average IDT strength of conditioned

specimens to the average IDT strength of unconditioned specimens, as shown in Equation 8.

𝑇𝑆𝑅 (%) =𝐼𝐷𝑇𝑤

𝐼𝐷𝑇𝐷× 100 (8)

where,

TSR = tensile strength ratio

IDTw = average indirect tensile strength for the conditioned set

IDTD = average indirect tensile strength for the unconditioned set

According to IDOT specifications, the TSR threshold is 85%. In the event the mix has a TSR

lower than 85%, the mixture is considered moisture susceptible or prone to stripping. Also, the

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minimum acceptable IDT strength is 60 psi (413.7 kPa) and 80 psi (551.6 kPa) for unmodified

and modified asphalt binder, respectively. The minimum IDT strength is applicable for both

unconditioned and conditioned specimens. IDOT uses 3 replicates for TSR. Hence, this study

complies with IDOT requirements. The TSR variability is high, the more tests run, the lower the

COV. However, in this study, three replicates were considered adequate with COV less than

10%.

3.3 MODIFIED LOTTMAN TEST

As previously explained, the Illinois modified AASHTO T283 test is a modified version

of the Lottman AASHTO T283 test. In this study, the conditioned set of specimens was further

conditioned for five FT cycles according to the following procedure:

1. The conditioned specimen air voids were saturated to a range of 70% to 80% under a vacuum

of 10 to 26 in Hg partial pressure (13 to 67 kPa absolute pressure).

2. The saturated conditioned specimen was then wrapped in a plastic film and placed inside a

plastic bag containing 0.61 ± 0.031 in3 (10 ± 0.5 mL) of water. The plastic

bag was sealed, and the specimen was placed in the freezer at a temperature of 0 ± 5°F (–18 ±

3°C) for at least 16 hrs.

3. The specimen was taken out from the freezer and the plastic film was immediately removed.

The specimen was then placed in a 140 ± 1.8°F (60 ± 1°C) water bath for 24 ± 1 hr.

4. Steps 2 and 3 represent one FT cycle. For three and five FT cycles, both steps were repeated

three and five times, respectively.

5. At the end of the last FT cycle (third or fifth), the conditioned specimens were transferred to a

77 ± 1.8°F (25 ± 1°C) water bath for 2 hr ± 10 min.

6. The conditioned set of specimens was tested for IDT strength (Figure 3.1).

3.4 DYNAMIC MODULUS TEST

Dynamic modulus (E*) is a fundamental linear viscoelastic material property used in the

Mechanistic Empirical Pavement Design Guide (MEPDG) as a primary material input for

pavement layers’ thickness design (Williams and Breakah 2010). Dynamic modulus is

considered one of the oldest mechanistic tests which was studied since the early 60’s but did not

become a standard test until the late 70’s (Papazian 1962). Dynamic modulus describes AC

response to sinusoidal loading conditions. The magnitude of the modulus is based on the AC

strength and degree of bonding between asphalt binder and aggregate (Bruce 1978). The

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behavior of AC can be represented by the dynamic modulus. Thus, dynamic modulus has a

significant correlation with field performance (Xu 2012). Dynamic modulus is capable of

describing the potential behavior of AC in resisting rutting and cracking (NCHRP 2004,

Williams and Breakah 2010).

The dynamic modulus test of AC samples will be conducted according to AASHTO T 342 at

temperatures of -10, 4, 21, 37, and 54oC and frequencies of 25, 10, 5, 1, and 0.1 Hz. Running at

different temperatures and frequencies ensures capturing the linear viscoelastic properties of AC

(Williams and Breakah 2010). Results from the different temperatures and frequencies are used

to develop a master curve which displays the AC properties over a wide range of reduced

temperatures or frequencies (Williams and Breakah 2010). The experimental setup for E* is

shown in Figure 3.2.

The complex modulus sample dimensions are 4.0 in (100 mm) in diameter and 5.9 in (150 mm)

in thickness. This sample is fabricated originally from a gyratory compacted sample with 5.9 in

(150 mm) in diameter and 7.1 in (180 mm) in thickness. The air void content of gyratory sample

is 7.0% ± 0.5%.

The dynamic modulus parameter was used in many studies to evaluate the AC moisture

susceptibility. The modulus was found to be inconsistent when used as a moisture damage

evaluator when compared with resilient modulus and maximum tensile strength (Bruce 1978).

However, other studies showed that dynamic modulus had the potential to evaluate asphalt

mixtures moisture susceptibility (Nadkarni et al. 2009; Solaimanian et al. 2003; Tseng and Lin

2013).

The master curve of dynamic modulus is considered proper tool to show the damage caused by

moisture (Williams and Breakah 2010). Generally, it was found out that moisture conditioning

results in reducing the AC stiffness (Tseng and Lin 2013; Williams and Breakah 2010; Xu 2012).

The impact of moisture conditioning on dynamic modulus is higher at high temperature/or low

frequencies (Williams and Breakah 2010).

3.5 AGING AND CONDITIONING

Typically, after mixing aggregate and asphalt binder, the mixture is placed in the oven to

simulate the short-term aging. In this study, two aging durations were considered: 1 hr at 311°F

(155°C) based on IDOT specifications and 4 hrs at 275°F (135°C) based on AASHTO

specifications (AASHTO R30-02).

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The samples prepared for the both Lottman and complex modulus tests were conditioned under

one of three conditioning levels: IDOT conditioning procedure, three FT cycles and five FT

cycles. In addition to the previous three conditioning levels, there was a separate set for each test

that was unconditioned.

Unconditioned set samples were only placed in a 25 ± 1°C (77 ± 1.8°F) water bath for 2 hrs ± 10

min prior to testing. Samples to be conditioned under IDOT conditioning procedure, three FT

and five FT were saturated by filling 70%–80% of air void volume with water. The IDOT

conditioning procedure consists of placing samples in a 60 ± 1°C (140±1.8°F) water bath for 24

± 1 hrs then for 2 hrs ± 10 min in a 25 ± 1°C (77 ± 1.8°F) water bath prior to testing. Each FT

cycle includes a minimum of 16 hrs freeze cycle at -18 3°C (0 5°F) followed by 24 1 hr

conditioning at 60 1°C (140 1.8°F) in water bath. After the last thawing cycle, the samples

were placed in 25 1°C (77 1.8°F) water bath for 2 hrs 10 min before testing.

For the experimental design, each mixture level test consists of two independent variables; aging

and conditioning. The aging variable consist of two levels (1 hr and 4 hrs) while the conditioning

variable consists of four variables (unconditioned, ILDOT conditioning, 3 FT, and 5 FT). In total

there are 8 groups (2x4) for each mixture level test. So no factorial design was needed.

Figure 3.3a and Figure 3.3b illustrate the experimental matrix for Lottman test and complex

modulus test for each asphalt mix, respectively.

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Chapter 3 Figures and Tables

Figure 3.1 Indirect tensile (IDT) strength testing.

Figure 3.2 Experimental setup of dynamic modulus test.

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(a)

(b)

Figure 3.3 Experimental matrix for each asphalt mix: (a) Lottman test; (b) complex modulus test.

Modified AASHTO T-283

1 hr @ 155°C

Unconditioned IDOT Conditioning

3 FT 5 FT

4 hrs @ 135°C

Unconditioned IDOT Conditioninig

3 FT 5 FT

Dynamic Modulus

1 hr @ 155°C

Unconditioned IDOT Conditioning

3 FT 5 FT

4 hrs @ 135°C

Unconditioned IDOT Conditioninig

3 FT 5 FT

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CHAPTER 4 COMPONENT-LEVEL CHARACTERIZATION

4.1 INTRODUCTION

Seven types of asphalt binder, as well as two types of aggregate, were evaluated by

means of four component-level tests. The seven asphalt binders shared the same neat asphalt

binder, PG 64-22 (control binder). The seven asphalt binders are the control, control with LAS,

control with HL, control with SBS, control with SBS and LAS, control with polyphosphoric acid

PPA and HL, and control with RAP. The aggregates were dolomitic limestone and lime. The

four component-level tests were the surface free energy (SFE) test, direct adhesion test (DAT),

blister test (BT), and dynamic mechanical analyzer (DMA).

4.2 MATERIALS

The asphalt binder, LAS, HL, SBS, and PPA are discussed in Chapter 3. Limestone and

lime aggregates were imported from Kankakee, IL and Lime Mineral Association, respectively.

4.3 ADHESION TESTS

Adhesion is considered a major parameter to be measured and evaluated when studying

moisture susceptibility of asphalt mixtures (Bhasin 2006; Canestraria et al. 2010; Copeland

2007; Hanz et al. 2007; Moraes et al. 2011). Various tests are proposed in the literature to test

adhesion bonding between asphalt binder and aggregate. Surface free energy (Cheng 2002),

bitumen bond strength (BBS) (Moraes et al. 2011), modified dynamic shear rheometer strain

sweep test (Cho 2008), and pneumatic adhesion tensile tester (PATTI) (Youtcheff and Aurilio

1997) are all examples of adhesion tests. Many of the current tests show promising results in

finding compatible aggregate-asphalt binder combinations capable of resisting moisture damage.

Both asphalt binder and aggregate characteristics influence the bonding between them (Copeland

2007; Moraes et al. 2011; Tarrer and Wagh 1992). Three major mechanisms are responsible for

the bonding between aggregate and asphalt binder, namely, chemical reaction, physical adhesion,

and mechanical bonding (Bhasin 2006; Ishai and Craus 1977; Rice 1958).

Three adhesion tests, surface free enery, DAT and BT, are available at the Advanced

Transportation Engineering and Research Laboratory (ATREL) in UIUC. The DAT and BT

were originally developed to measure the adhesion properties for hot-poured crack sealant. In

this study, the applicability of these tests to measure the adhesion properties of asphalt binder

was evaluated.

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4.3.1 Surface Free Energy

Bond energy between asphalt binder and aggregate, asphalt binder viscoelastic properties,

and distribution of internal structure all influence the overall performance of asphalt mixture

(Little and Bhasin 2006; Masad et al. 2006b).

Failure of a bituminous mix caused by moisture can be attributed to adhesive and/or cohesive

damage within the mix. Adhesion between aggregate and asphalt binder can be described as a

fundamental characteristic. Fundamental adhesion refers to the forces that exist on the surface (to

form the interfacial layer) and affect the bond strength between asphalt and aggregate (Wei and

Zhang 2012). The tendency of these forces to form a surface is known as “surface energy,”

which is defined as the amount of work required to form a unit area of the surface in vacuum.

Surface energy is a more general term compared with surface tension as it can be applied to both

solid and liquids (Lobato 2004). Surface energy has the dimension of energy per unit area.

Surface tension and surface energy are the same for liquids (Good 1979; Lobato 2004).

However, surface energy represents a better physical significance for solids because forming

addition surface area of any solid requires the application of work (Good 1979; Lobato 2004).

The SFE of any non-metallic material has two components: a nonpolar/dispersive element

(apolar intermolecular forces such as Lifshitz–van der Waals, LW, forces) and a polar element

(monopolar acid–base, AB, interactions such as hydrogen bonding) (Fowkes 1962; Lobato 2004;

Howson et al. 2007). Lifshitz–Van der Waals forces consist of London dispersion forces, Debye

induction forces, and Keesom orientation forces. Good and Van Oss (1988) further categorized

the polar component as Lewis acid and Lewis base surface parameters. A linear combination of

these forces to calculate total SFE value is shown in Equation 9:

ΓTotal = ΓLW + ΓAB = ΓLW + 2√Γ+Γ− (9)

where,

ΓTotal = total SFE

ΓLW = nonpolar component

ΓAB = acid-base component

Γ+ = Lewis acid component

Γ- = Lewis base component

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This theory is also known as the three-component theory or acid–base theory, which is preferred

over the Fowkes two-component theory because it better clarifies the interactions between

different components in a mix.

SFE represent a material property which relates to the asphalt mixture fatigue cracking and

moisture sensitivity (Howson et al. 2007). Several studies show a good correlation between SFE

and moisture damage (Bhasin et al. 2006; Little and Bhasin 2006; Masad et al. 2006b). However,

the fracture energy measured from the mechanical testing introduces factors such as heat

dissipation, acoustic emissions, and plastic deformation which cannot be considered in fracture

energy measured from surface free energy (Howson et al. 2007).

Asphalt binder and aggregate SFE components were measured using a sessile drop device based

on contact angle measurement. The nomenclature for SFE components of asphalt binder and

aggregate are (ΓbLW, Γb

− and Γb+) and (Γ𝑠

LW, Γ𝑠− and Γ𝑠

+), respectively.

The concept of contact angle measurement was first introduced in 1805 by Thomas Young

(Zenkiewicz 2007). Determining the interaction energy existing between solids and liquids using

contact angle is still considered one of the most accurate methods (Lobato 2004; Zenkiewicz

2007). The sessile drop devices were used originally in various fields such as painting, mining

and coating (Koc and Bulut 2013).

In this research, a sessile drop apparatus (Figure 4.1), developed by Kyowa Interface Co. Ltd in

Japan, was used to measure material contact angle. UIUC owns the latest version of this

instrument, from Drop Master Series, with a DM501/701 model for surface analysis. The

FAMAS (interface measurement and analysis system) software supplied with the device

measures the contact angles at a specified time interval as well as other details, such as drop

volume and drop dimensions. Measuring the contact angle using the sessile drop device is

considered one of the most popular and convenient methods (Bahramian 2012; Koc and Bulut

2013; Lobato 2004; Wei and Zhang 2012). In addition, the need for small quantities from both

the solid and liquid materials is another sessile drop device advantage (Lobato 2004). On the

other hand, the major drawback of the sessile drop device is being subjective and operator

dependent (Lam et al. 2002; Lobato 2004; Neumann and Good 1979).

To determine surface energy using the sessile drop equipment, a specific set of probe liquids is

required. The probe liquids are based on the surface tension value of liquids compared with the

bitumen or aggregate used (surface tension value of substrate < surface tension of probe liquids

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used) (Little and Bhasin 2006; Lobato 2004). In this context, water, glycerol, and diiodomethane

were selected to test the SFE components for the various types of asphalt bitumen and aggregate.

When using the automatic dispenser, the volume of the droplet is automatically administered by

the software, and an image of the droplet on the bitumen surface is captured by the FAMAS

software to record the advancing contact angle as an average value and the standard deviation for

three observations. The measured contact angle of the probe liquid droplet on the substrate

represents an average of the angles measured on the left and right of the placed droplet, as shown

in Figure 4.2.

Wei and Zhang (2012) measured the SFE for aggregate and asphalt binder using the sessile drop

device. Their results show that the sessile drop device is capable of ranking asphalt binder-

aggregate combinations based on their SFE and work of adhesion. It should be noted that the

aggregate SFE measured by the sessile drop device is less than the SFE measured using the

universal sorption device because of the equilibrium spreading pressure (Wei and Zhang 2012).

Despite that, the sessile drop device is still capable of ranking aggregate based on their SFE (Wei

and Zhang 2012).

When preparing bitumen and aggregate samples for contact angle measurement, a smooth, clean,

rigid, homogenous, and horizontal surface of the specimen must be maintained (Lam et al. 2002;

Lobato 2004). For that purpose, special molds of aluminum were fabricated with a square base

plate of 2 × 2 in (50 × 50 mm) cross section and a height of 0.2 in (5 mm) to prepare asphalt

binder samples. Clips were affixed at all four sides, as shown in Figure 4.3, to prevent asphalt

binder flow and maintain the proper shape and a level surface.

The asphalt binder sample was heated until it reached a flowable state. The sample was then

transferred to aluminum cups that could be bent to direct the flow of the asphalt binder.

Meanwhile, side components of molds were fixed onto base plates using binder clips. Hot

asphalt binder was poured in each mold such that a horizontal surface was formed. After 24 hr,

the side components of the molds were removed and the asphalt binder sample was ready for

measurement on the sessile drop device.

Squared aggregate samples were prepared to a thickness of 0.2 in (5 mm), see Figure 4.4. The

aggregate surfaces were polished smooth and horizontal as previously mentioned. Aggregate

SFE testing procedure is similar to the one performed on asphalt binder samples.

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The contact angle measured between a probe liquid and a solid substrate (in this case asphalt

binder or aggregate) can be linked to SFE components through the following Young–Dupré

relation (Equation 10):

ΓLTotal(1 + cosθ) = 2 × √Γm

LWΓLLW + 2 × √Γm

−ΓL+ + 2 × √Γm

+ΓL− (10)

where:

ΓmLW, Γm

− and Γm+ : SFE components of solid substrate material (asphalt binder or aggregate)

ΓLTotal, ΓL

LW, ΓL+ and ΓL

−: SFE total and components of liquid solvent

θ: contact angle

A minimum of three liquids is required to determine the three unknown SFE components of

asphalt binder and aggregate. Based on the concept of surface energy, certain thermodynamic

variables are used to describe the sensitivity of an asphalt mixture to moisture, which are

discussed in the following sections.

4.3.1.1 Work of Adhesion

Work of adhesion (Ws,ba ) is the amount of work required to separate two materials (i.e.,

aggregate and asphalt binder) at the interface. For two materials in contact with each other, the

energy required to separate them is equal to the sum of individual surface energies of the

components reduced by a portion of the intermolecular forces existing on the interface.

According to the acid–base theory, work of adhesion is calculated as shown in Equation 11

(Wasiuddin et al. 2007a; Cheng et al. 2003; Bhasin et al. 2007a; Bhasin et al. 2007b; Bhasin and

Little 2009):

Ws,ba = 2√Γs

LWΓbLW + 2√Γs

+Γb− + 2√Γs

−Γb+ (11)

4.3.1.2 Work of Cohesion

Work of cohesion (for asphalt binder) (Wb,ba ) is defined as the amount of work done on a

system to reversibly separate a column (liquid/solid) of unit area into two new surfaces (each of

unit area). It is given as surface energy value times the amount of new surfaces created, as shown

in Equation 12 (Bhasin et al. 2007a):

Wb,ba = 2Γb

LW + 4√Γb+Γb

− (12)

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Figure 4.5 illustrates the concepts of work of adhesion and cohesion in more detail.

4.3.2 Direct Adhesion Test

The direct adhesion test (DAT) evaluates adhesion at the asphalt binder–aluminum

interface. Aluminum was selected because it is compatible with asphalt binder, easily available,

and has low diffusion, controllable roughness, high resistance to extreme temperatures, and a

thermal coefficient similar to that of aggregates (Fini and Al-Qadi 2011). In addition, the surface

energy of aluminum is relatively low compared with that of aggregate.

The assembly consisted of two half-cylinder aluminum parts 1 in (25 mm) in diameter and 0.47

in (12 mm) long, as shown in Figure 4.6. A half-cylinder mold, with the upper part open, was

placed between the aluminum parts on a level surface. The asphalt binder poured into the mold

was therefore confined between the two end pieces. A pre-debonded area in the form of a crack

at one side of the asphalt binder–aluminum interface was created to ensure that adhesive failure

occurred and to define the failure’s location. To create the crack, a 1 x 0.08 in (25 × 2 mm) shim

was placed on the upper edge of the aluminum piece on the fixed side of the direct tension test

fixture. The shim was removed after the asphalt binder was poured and cooled, leaving a notch

0.08 in (2 mm) deep, which is the initial failure location at the aluminum–asphalt binder

interface.

The two half-cylinder aluminum parts were assembled. To facilitate separating the asphalt binder

sample after it cooled down, the mold and the shim were sprayed with a silicone based release

agent. The assembly was secured and placed on a base plate. The heated asphalt binder was

poured into the mold from one corner to avoid formation of air bubbles. The sample was left for

1 hr of annealing at room temperature, after which the specimen was trimmed and placed in a

cooling bath for 15 min. The specimen was then removed from the bath, demolded, and placed

back in the bath for another 45 min to allow for equilibration before testing.

The output of the DAT is a curve representing load versus displacement. The maximum load,

Pmax, and bond energy, E, can be calculated for each asphalt binder–aluminum pair, as shown in

Figure 4.7. The higher the Pmax and E, the better the adherence properties of the asphalt binder.

Using the setup described above, asphalt binder was tested at a temperature of 39.2°F (4°C). The

area under the load-displacement curve can be divided by the contact cross area to calculate the

energy. Because a debonded area was created and the failure path was defined, no energy was

dissipated in crack initiation, which helped obtain consistent results.

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Al-Qadi et al. (2008) found that DAT results had a high average coefficient of variation (COV).

DAT results are very sensitive to test variables. Thus, careful consideration should be given to

specimen preparation, pouring and testing temperature, and viscosity. This sensitivity to

variables is the main reason behind the relatively high COV.

4.3.3 Blister Test

Another adhesion test used is blister test (BT); which allows measuring interfacial

fracture energy. The interfacial fracture energy is a geometry-independent engineering term

defined as the required energy to debond a unit area at the interface (Al-Qadi et al. 2008; Bennett

et al. 1974; Penn and Defex 2002). Adhesion is also measured between asphalt binder and an

aluminum substrate because of the same aforementioned reasons. However, the aluminum

substrate for the BT is completely different from that of the DAT; the former is a donut-shaped

annular disk, as shown in Figure 4.8. One of the reasons behind this being an attractive test is

having a stable interface (Al-Qadi et al. 2008). Williams (1969) was the first to develop the BT;

modification was then introduced to BT by Burton et al. (1971). A layer of asphalt binder is

poured on top of the aluminum disk. Alcohol is injected using a servo-hydraulic pump through

the orifice in the aluminum substrate, resulting in a blister formation in asphalt binder, as shown

in Figure 4.9. The blister keeps growing with increasing alcohol pressure until full separation

occurs between asphalt binder and the aluminum disk. The pressure and blister height are

recorded for each asphalt binder as functions of time. Both outputs are used to calculate the

asphalt modulus and the interfacial fracture energy (IFE). The modulus and the IFE are sufficient

to predict the adhesive failure (Al-Qadi et al. 2008).

The variability in the BT results is almost similar to DAT. Therefore, careful consideration

should be considered for all test variables especially surface preparation in order to obtain

repeatable IFE results (Al-Qadi et al. 2008; Bennett et al. 1974).

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Chapter 4 Figures and Tables

Figure 4.1 Sessile drop device.

Figure 4.2 Contact angle measurement.

Figure 4.3 SFE asphalt binder sample.

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47

Figure 4.4 Aggregate SFE sample.

Figure 4.5 SFE-based evaluation parameters: work of adhesion (top); work of cohesion (bottom).

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Figure 4.6 DAT specimen fixture.

Figure 4.7 Typical DAT results (Al-Qadi et al. 2008).

Figure 4.8 Blister sample aluminum substrate with and without asphalt binder.

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Figure 4.9 Schematic showing blister mechanism (Al-Qadi et al. 2008).

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CHAPTER 5 MIXTURE-LEVEL TESTS: RESULTS AND DISCUSSION

5.1 INTRODUCTION

Two mechanisms are associated with moisture damage: loss of cohesion and loss of

adhesion (Cheng et al. 2003, Izzo and Tahmoressi 1999, Peiwen and Hong Ying 2006, Sebaaly

et al. 2007, Wasiuddin et al. 2007a). In the loss of cohesion, water softens the asphalt binder,

resulting in a reduction in overall mixture strength. The loss of adhesion occurs when water

penetrates between the aggregate and binder film (along with chemo and physical reactions),

which results in stripping. Different distresses are caused as a result of these two mechanisms,

such as rutting, raveling, fatigue cracking, and bleeding (Sebaaly et al. 2003, Wasiuddin et al.

2007a). Thus, moisture damage is defined as the loss of pavement strength and durability caused

by moisture (Bhasin et al. 2007b, Huang et al. 2009).

In the field, pavements are subject to several environmental conditions, which eventually alter

the properties of asphalt pavement (Terrel and Al-Swailmi 1994). This alteration affects the

moisture sensitivity of asphalt pavement. Climate is one of the factors affecting moisture

sensitivity of asphalt mixtures, in addition to aggregate and asphalt binder properties, mixture

characteristics, pavement design, and traffic loading (Bhasin et al. 2007b, Chen et al. 2006,

Mallick et al. 2005, Peiwen and Hong Ying 2006, Sebaaly et al. 2003, Sebaaly et al. 2007).

Pavements are subject to temperature and moisture which trigger oxidation and possibly multiple

freezing and thawing cycles (climatic region dependent).

The fact that moisture damage occurs in the early phases of the service life indicates the

significance of short-term aging and its relevance to the moisture sensitivity of asphalt mixes.

Short-term aging represent the period starting from production and ending with construction

(Bell 1989, Lee et al. 2007). Simulating short-term aging in the lab is a challenge. Several

researchers and DOTs developed specific durations to simulate short-term aging. In addition,

each DOT developed a moisture conditioning procedure to simulate the conditioning that the

asphalt mixture is subjected to in the field.

To mitigate moisture damage, transportation agencies typically add additives and/or modifiers to

moisture-susceptible asphalt mixes (Huang et al. 2009, Lu and Harvey 2006, Peiwen and Hong

Ying 2006, Sebaaly et al. 2007). The additives and modifiers are either added to the aggregate or

asphalt binder to enhance the bonding between them (Chen et al. 2006).

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To recognize moisture damage, the moisture susceptibility of asphalt mixtures must be evaluated

(Izzo and Tahmoressi 1999). This is usually achieved by testing the mixtures or their

components (component level). There are several types of tests that evaluate moisture

susceptibility of asphalt mixtures (Tarefder and Zaman 2009). Each test introduces a unique

conditioning procedure that subjects the tested sample to the influence of moisture. The modified

Lottman AASHTO T 283 test is a typical moisture susceptibility test (Birgisson et al. 2007, Caro

et al. 2008b).

Studying moisture damage presents two main challenges: First, moisture damage occurs in the

early phases of pavement service life, resulting in premature failure and, consequently, in billions

of dollars spent on maintenance and reconstruction (Caro et al. 2008a, Izzo and Tahmoressi

1999). Second, the tests have limited ability to simulate field conditions (Caro et al. 2008a). New

approaches have been developed to evaluate asphalt concrete moisture damage, including

analytical methods and laboratory tests conducted at the component level (binder and aggregate).

In this study, one aggregate, control binder, two additives, two modifiers, and a recycled asphalt

pavement (RAP) were used. The aggregate is dolomitic limestone; the control binder has a

performance grade (PG) of 64-22; the additives are liquid anti-stripping (LAS) agent and

hydrated lime (HL); and the modifiers are polyphosphoric acid (PPA) and styrene butadiene

styrene (SBS). Seven mixes were prepared from the control binder and selected additives,

modifiers and RAP: control mix, control mix with LAS, control mix with HL, control mix with

SBS, control mix with SBS and LAS, control mix with PPA and HL, and control mix with RAP.

In this study, two mixture-level tests were adopted to evaluate moisture resistance of asphalt

mixes: modified Lottman test (AASHTO T283) and complex modulus test (AASHTO T 342).

Two aging durations and four conditioning periods were considered for the mixture-level tests.

The two aging durations are 1 hr at 155°C (311°F) and 4 hrs at 135°C (275°F). The conditioning

periods are unconditioned (dry), IDOT conditioning, three freezing and thawing (FT) cycles, and

5 FT cycles. The materials used including additives and modifiers are presented in Chapter 2.

Laboratory tests and conditioning of specimens are presented in Chapter 3.

5.2 RESULTS AND DISCUSSION

5.2.1 Illinois Modified Lottman Test (AASHTO T 283)

Table 5.1 shows the results for N90 control mix. The tensile strength ration (TSR) of the

N90 control mix is less than 85.0%. Based on IDOT specifications, the mix is moisture

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susceptible. In addition, the tensile strength for the conditioned set was less than the 60 psi

threshold while the unconditioned tensile strength was barely above the same threshold, which

indicates that N90 control mix is also weak.

5.2.2 Modified Lottman Test (AASHTO T 283)

Table 5.2 and Table 5.3 present the IDT and TSR results for all mixes tested with

modified Lottman test under the various adopted aging and conditioning durations, respectively.

Figure 5.1 and Figure 5.2 show a graphical representation of the results included in Table 5.2 and

Table 5.3, respectively.

The modified Lottman test, as mentioned earlier, results in two parameters; namely IDT strength

for unconditioned and conditioned sets and TSR. IDT describes the AC mix strength; while TSR

describes the ability of AC mix to resist moisture. Both parameters are important to evaluate the

performance of AC mix. IDOT specifies 60 psi and 80 psi as the IDT threshold for unmodified

and modified AC mixes, respectively. AASHTO specifies TSR threshold as 80% while IDOT

TSR threshold is 85%. It is recommended to design AC mixes with IDT (before and after

conditioning) and TSR values surpassing the thresholds. It is not necessary that both parameters

provide the same ranking when comparing AC mixes. This is obvious, for example, when

comparing Control+LAS with either Control+SBS or Control+RAP. Control+LAS had lower

IDT than Control+RAP; but higher TSR. Theoretically this indicates that Control+LAS had

lower strength, but higher moisture resistance in comparison to the AC mix with RAP.

Table 5.2 shows that IDT strength of asphalt mixes after 4 hrs of aging is always higher than that

after 1 hr of aging, despite the conditioning period. The IDT strength of asphalt mixes decreases

with more conditioning within the same aging period. The addition of RAP to the control mix

resulted in the highest IDT strength for all cases except at 3 and 5 FT after 4 hrs of aging. The

RAP, additives, and modifiers considered in this study improved the IDT strength with respect to

the control mix except in the case of LAS at 1h (unconditioned), where significant softening was

observed. This softening agrees with literature reports (Berthelot et al. 2010). The softening

influence caused by LAS seems to diminish with more aging as shown in the IDT 4 hrs

(unconditioned) state. It seems that more aging results in an increase in mixture stability when

LAS is added. However, when conditioning was introduced (IDOT, 3 FT cycles, and 5 FT

cycles), the mix with LAS produced higher IDT strength compared with the control mix. This

indicates the ability of the LAS additive to better sustain the mix strength after conditioning.

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The IDT strength reduction rate with the increase in conditioning for the 1 hr aged mix with LAS

is minimal, while for mixes with LAS after 4 hrs aging, the reduction rate is greater. In other

words, the negative impact of moisture on mixes with LAS increases with aging. This could be

attributed to heat instability, which is one documented drawback associated with the use of LAS

additive (Anderson and Dukatz 1982; Khosla and Harikrishnan 2007).

The influence of LAS additive when added to the SBS-modified mix after 1 hr and 4 hrs aging in

the unconditioned state showed no significant alteration compared with the SBS mix. This means

that the polymer influence overcomes the LAS softening influence especially at 1 hr aging. On

the other hand, the IDT measured for the 1 hr and 4 hrs aged mixes with SBS+LAS after IDOT,

3 FT and 5 FT conditioning was generally higher compared with the mixes with SBS only;

especially after the 5 FT cycles. This indicates that the LAS influence overcomes the SBS effect

because the IDT strength is retained after excessive conditioning. SBS+LAS ends up as a stiff

mix with a greater ability to resist moisture.

PPA is a modifier used to reduce the rate of aging in asphalt mixtures; it also modifies the

performance grade of asphalt binder (Huang et al. 2011). On the other hand, HL is commonly

used to reduce moisture susceptibility and increase strength of asphalt mixes (Birdsall 1999,

Hicks and Scholz 2001; Kennedy and Anagnos 1984; Khosla and Harikrishnan 2007; Lesueur

and Little 1999; Little and Epps 2011; Mohammad et al. 2000; Petersen et al. 1987). The

comparison between PPA+HL mix and HL mix resulted in two interesting findings (see Table

5.2). First, after unconditioned, IDOT conditioning and 3 FT cycles, the mix with PPA+HL had

higher and lower IDT strengths at 1 hr and 4 hrs aging, respectively. This shows an

interchanging effect of PPA at 1 hr and 4 hrs aging. At 1 hr aging, PPA performed more as a

modifier resulting in a stiffer mix, while at 4 hrs PPA reduced the aging rate, thus resulting in a

softer mix. Second, there is no significant difference in the IDT strength between both mixes

after 5 FT cycles despite the aging duration. It seems that with excessive conditioning both

PPA+HL and HL mixes fail regardless of the properties of PPA and HL.

Table 5.3 TSR Values for Asphalt Mixes at Different Aging and Conditioning Periods shows

that RAP and the additives and modifiers considered in this study generally improved moisture

resistance in all cases as compared with the control mix. The mix with SBS+LAS showed the

best moisture resistance, followed by the mix with LAS. This indicates that using LAS with

modified and unmodified mixes eventually improves the moisture resistance of these mixes. HL

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also improved moisture resistance, but it was not as efficient as LAS especially when added to

PPA.

The moisture resistance of asphalt mixes using the modified AASHTO T283 was evaluated after

short-term aging. Several studies reported that HL shows better performance (higher moisture

resistance) after long-term aging compared with LAS additive (Lu and Harvey 2006). This was

not verified in this test, but it was evaluated in the component testing.

Generally, TSR is higher after 1 hr than TSR after 4 hrs aging. In other words, moisture

resistance of asphalt mixes drops with aging. This agrees with previous work that found that

sensitivity to moisture damage increases with aging (Molenaar et al. 2010). This was not the case

for HL mix after IDOT and 3 FT conditioning and the control mix in all cases where sensitivity

to moisture damage decreased with aging (further statistical analysis will be conducted in the

following section).

TSR decreases with more conditioning after the same aging duration. In other words, the

moisture susceptibility of asphalt mixes increases with more conditioning.

It is well known in the literature that adding SBS or RAP increases the stiffness and strength of

asphalt mixtures (Aurangzeb et al. 2012, Bahia et al. 2001, Freeman et al. 1997). In this study,

the addition of 50% RAP to the control mix produced the highest IDT strength in almost all

cases compared with the other mixes regardless of aging and conditioning durations, see Table

5.2. The addition of SBS to control also increased the strength in comparison with the other

mixes, expect for the RAP mix. However, this increase occurred only at the unconditioned and

IDOT states after that the SBS-modified mix strength deteriorated under the impact of extensive

moisture conditioning. Despite the increase in strength, SBS and RAP were less effective in

reducing moisture susceptibility.

Therefore, the results shown in Table 5.2 and Table 5.3 TSR Values for Asphalt Mixes at

Different Aging and Conditioning Periods indicate that only LAS and HL improved moisture

resistance. The improvement resulting from the addition of LAS to the control mixes is irrelevant

to whether the mix is modified or unmodified. On the other hand, HL was more efficient in

resisting moisture as compared to its efficiency when added to the PPA-modified asphalt mix.

RAP and modified mixes (SBS mix and PPA+HL mix) were not efficient in reducing moisture

susceptibility.

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In the following section, the Statistical Package for the Social Sciences (SPSS) software was

used to statistically analyze the IDT and TSR results for each mix at all aging and conditioning

stages.

5.2.2.1 Statistical Analysis

Table 5.4 to Table 5.10 display the IDT statistical analysis conducted using SPSS

software for control, LAS, HL, PPA+HL, SBS, SBS+LAS and RAP mixes, respectively. Table

5.11 to Table 5.17 display the TSR statistical analysis conducted using SPSS software for

control, LAS, HL, PPA+HL, SBS, SBS+LAS and RAP mixes, respectively.

The statistical analysis in Table 5.4 through Table 5.10 show a significant difference between

IDT measured after 1 hr and 4 hrs aging for all mixes at the unconditioned (dry) and IDOT (IL)

conditioning stage, except for mixes with RAP. However, after 3 FT cycles, the mixes could be

categorized into two groups: soft mixes (control, LAS, and HL) and stiffer mixes (PPA+HL,

SBS, SBS+LAS, and RAP). There was a significant difference between IDT 1 hr and IDT 4 hrs

for the soft mixes, but not for stiffer mixes. As for the 5 FT cycles, both soft and stiff mixes

showed insignificant difference between IDT 1 hr and IDT 4 hrs. This suggests that the influence

of aging on IDT strength diminishes with extensive conditioning.

The results in Table 5.11 through Table 5.17 show that aging duration (1 hr vs 4 hrs) had no

influence on the moisture susceptibility of asphalt mixes after IDOT and 3 FT conditioning. The

only mix influenced by aging duration after IDOT and 3 FT conditioning is the mixture with

PPA+HL and mixture with RAP, respectively. In addition, the moisture sensitivity (TSR) of

PPA+HL mix aged with 4 hrs did not significantly drop with increased conditioning which was

not the case for the mixes with PPA+HL aged for 1 hr.

There was no significant difference between TSR at 1 hr and 4 hrs for control, mixes with

PPA+HL, SBS, or SBS+LAS after 5 FT conditioning. However, there was a significant

difference in moisture susceptibility for mixes with LAS, HL, or RAP after 5 FT conditioning

because of the variation in aging.

The statistical analysis shows that aging duration becomes ineffective when moisture

susceptibility is evaluated after 3 FT cycles or less. However, if moisture susceptibility is to be

evaluated after 5 FT cycles, then it is recommended to age the mix for 4 hrs because moisture

susceptibility would then be higher than after 1 hr aging.

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The above statistical analysis shows that moisture susceptibility can be best evaluated using the

modified Lottman test, if extensive conditioning is considered, at 4 hrs aging with 5 FT

conditioning. This finding is based on two observed facts: First, there was no significant

difference between 1 hr IDT and 4 hrs IDT with 5 FT conditioning; second, there was no

significant difference between 1 hr TSR and 4 hrs TSR with 5 FT conditioning for most asphalt

mixes considered in this study. In addition, the moisture susceptibility of asphalt mixes at 4 hrs

with 5 FT is higher compared with 1 hr with 5 FT. Testing at 4 hrs with 5 FT is more

conservative.

5.2.3 Complex Modulus (AASHTO T 342)

Figure 5.5(a), Figure 5.6(a), Figure 5.9(a), Figure 5.12(a), Figure 5.15(a), Figure 5.18(a),

and Figure 5.21(a) represent the complex modulus at 1 hr with all conditioning levels for control,

control with LAS, control with LimeD, PPA with LimeD, SBS, SBS with LAS, and 50% RAP

mixes, respectively. Figure 5.5(b), Figure 5.6(b), Figure 5.9(b), Figure 5.12(b), Figure 5.15(b),

Figure 5.18(b), and Figure 5.21(b) represent the complex modulus at 4 hrs with all conditioning

levels for control, control with LAS, control with LimeD, PPA with LimeD, SBS, SBS with

LAS, and 50% RAP mixes, respectively.

Figure 5.4(a), Figure 5.7(a), Figure 5.10(a), Figure 5.13(a), Figure 5.16(a), Figure 5.19(a), and

Figure 5.22(a) display a comparison between complex modulus measured after 1 hr and 4 hrs

aging at unconditioned level for control, control with LAS, control with LimeD, PPA with

LimeD, SBS, SBS with LAS, and 50% RAP mixes, respectively. Figure 5.4(b), Figure 5.7(b),

Figure 5.10(b), Figure 5.13(b), Figure 5.16(b), Figure 5.19(b), and Figure 5.22(b) display a

comparison between complex modulus measured after 1 hr and 4 hrs aging at IDOT conditioning

level for control, control with LAS, control with LimeD, PPA with LimeD, SBS, SBS with LAS,

and 50% RAP mixes, respectively.

Figure 5.5(a), Figure 5.8(a), Figure 5.11(a), Figure 5.14(a), Figure 5.17(a), Figure 5.20(a), and

Figure 5.23(a) display a comparison between complex modulus measured after 1 hr and 4 hrs

aging at 3 FT conditioning level for control, control with LAS, control with LimeD, PPA with

LimeD, SBS, SBS with LAS, and 50% RAP mixes, respectively. Figure 5.5(b), Figure 5.8(b),

Figure 5.11(b), Figure 5.14(b), Figure 5.17(b), Figure 5.20(b), and Figure 5.23(b) display a

comparison between complex modulus measured after 1 hr and 4 hrs aging at 5 FT conditioning

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level for control, control with LAS, control with LimeD, PPA with LimeD, SBS, SBS with LAS,

and 50% RAP mixes, respectively.

Figure 5.5(a), Figure 5.6(a), Figure 5.9(a), Figure 5.12(a), Figure 5.15(a), Figure 5.18(a), Figure

5.21(a), Figure 5.5(b), Figure 5.6(b), Figure 5.9(b), Figure 5.12(b), Figure 5.15(b), Figure

5.18(b), and Figure 5.21(b) show that additional conditioning results in a drop in stiffness despite

aging duration (1 hr and 4 hrs). The difference in stiffness between the conditioning levels is

obvious at low frequency (high temperature) while no significant difference is observed at the

high frequency (low temperature). Williams and Breakah 2010 also reported that the impact of

moisture conditioning on dynamic modulus is higher at high temperature/or low frequencies.

It should be noted that the difference between the master curves due to conditioning at same

aging duration is insignificant, which indicates that the dynamic modulus is not sensitive to

moisture conditioning.

Figure 5.4(a), Figure 5.7(a), Figure 5.10(a), Figure 5.13(a), Figure 5.16(a), Figure 5.19(a), Figure

5.22(a), Figure 5.4(b), Figure 5.7(b), Figure 5.10(b), Figure 5.13(b), Figure 5.16(b), Figure

5.19(b), Figure 5.22(b), Figure 5.5(a), Figure 5.8(a), Figure 5.11(a), Figure 5.14(a), Figure

5.17(a), Figure 5.20(a), Figure 5.23(a), Figure 5.5(b), Figure 5.8(b), Figure 5.11(b), Figure

5.14(b), Figure 5.17(b), Figure 5.20(b), and Figure 5.23(b) show that stiffness after 4 hrs aging is

higher than the stiffness measured after 1 hr aging. However, the difference in stiffness after 4

hrs aging and 1 hr aging is insignificant in the modified mixes (PPA+LimeD, SBS and

SBS+LAS) and RAP mix. This was not the case for the unmodified mixes (control,

control+LAS, and control+LimeD).

Figure 5.24 to Figure 5.31 display a comparison between the stiffness of mixes at multiple aging

and conditioning levels. The mix with RAP seems to produce the highest stiffness amongst the

asphalt mixes at all aging and conditioning levels. It is difficult to rank and evaluate the effect of

modifiers and additives at the different aging and conditioning levels for the other mixes.

In summary, Figure 5.5 to Figure 5.31 show that the dynamic modulus is:

1. Insensitive to the increase in conditioning period at the same aging duration; but sensitive

to aging for the unmodified compared with the modified and RAP mixes.

2. Insensitive to binder type (additives and modifiers) at aging and conditioning

combinations.

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The dynamic modulus is typically measured under compression sinusoidal loading (compression

mode). Compression loads are usually supported by the aggregate skeleton (Alshamsi 2006, Wu

et al. 2012). In asphalt mixes, aggregate typically represents 90%-95% by weight, which stands

for 75%-85% of the volume (Roberts et al., 2002). The aggregate governs stiffness of the asphalt

mix in compression; especially at low frequency (high temperature) (Lundy et al. 2005, Swamy

and Daniel 2012, Wu et al. 2012).

The master curves in Figure 5.5(a) are for the same mix (i.e., same aggregate structure) and the

same aging duration. Each master curve in Figure 5.5(a) is measured under a different

conditioning status. It is very likely that the conditioning applied in this study did not

significantly affect the properties and characteristics of the aggregate structure. This explains the

insensitivity of dynamic modulus to conditioning in Figure 5.5(a). The same applies to Figure

5.6(a), Figure 5.9(a), Figure 5.12(a), Figure 5.15(a), Figure 5.18(a), Figure 5.21(a), Figure 5.5(b),

Figure 5.6(b), Figure 5.9(b), Figure 5.12(b), Figure 5.15(b), Figure 5.18(b), and Figure 5.21(b).

All mixes in this study, except for the RAP mix, share the same aggregate structure. This

explains why the RAP mix generated different results compared with the other mixes, as shown

in Figure 5.24 to Figure 5.31, as well as the inability to distinguish and rank between the other

mixes.

The impact of asphalt binder becomes obvious when aging durations are compared (1 hr vs 4

hrs) at the same conditioning level. The difference in stiffness between 4 hrs aging and 1 hr

aging is insignificant for modified mixes and RAP mix (see Figure 5.13(a), Figure 5.16(a),

Figure 5.19(a), Figure 5.22(a), Figure 5.13(b), Figure 5.16(b), Figure 5.19(b), Figure 5.22(b),

Figure 5.14(a), Figure 5.17(a), Figure 5.20(a), Figure 5.23(a), Figure 5.14(b), Figure 5.17(b),

Figure 5.20(b), and Figure 5.23(b)) while it is significant for the unmodified mixes (see Figure

5.4(a), Figure 5.7(a), Figure 5.10(a), Figure 5.4(b), Figure 5.7(b), Figure 5.10(b), , Figure 5.5(a),

Figure 5.8(a), Figure 5.11(a), Figure 5.5(b), Figure 5.8(b), Figure 5.11(b)). In other words, the

stiffer the asphalt binder, the less the difference between dynamic modulus due to aging.

Therefore, the dynamic modulus is sensitive to aging when using soft binders (keeping the same

aggregate structure). The impact of aging is higher on soft binders compared with modified or

stiff binders.

Overall findings indicate that the dynamic modulus is not effective for evaluating moisture

damage in asphalt mixes because it is not sensitive to moisture conditioning. This finding agrees

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with other studies, such as Bruce (1978) who found that the modulus was inconsistent when used

as a moisture damage evaluator as compared with the resilient modulus and maximum tensile

strength.

5.3 SUMMARY

This chapter focuses on evaluating the influence of several additives, modifiers and RAP

on the moisture susceptibility of asphalt mixes by employing two mixture-level test, namely;

modified AASHTO T-283 and dynamic modulus tests. The moisture susceptibility was evaluated

under various aging and conditioning durations.

The results from modified AASHTO T-283 test indicate that LAS and HL improved moisture

resistance. LAS improvement was irrelevant whether the mix is modified or unmodified. HL was

more efficient in resisting moisture as compared to its efficiency when added to the PPA-

modified asphalt mixes. RAP and modified mixes (mixes with SBS or with PPA+HL) were not

efficient in reducing moisture susceptibility. Analyzing modified AASHTO T-283 results

statistically via SPSS point out that moisture susceptibility can be best evaluated using the

modified Lottman test, if extensive conditioning is considered, at 4 hrs aging with 5 FT

conditioning. On the other hand, the master curve obtained from the dynamic modulus test found

to be not as effective as tensile strength for evaluating moisture damage in asphalt mixes. This is

because master curve was found insensitive to moisture conditioning.

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Chapter 5 Figures and Tables

Figure 5.1 Indirect tensile (IDT) strength results for asphalt mixes at different aging and

conditioning periods

Figure 5.2 Tensile strength ratio (TSR) values for asphalt mixes at various aging and

conditioning periods

0

20

40

60

80

100

120

140

Control LAS HL PPA+HL SBS SBS+LAS RAP

IDT

(psi

)

Uncond. 1hr IDOT 1hr 3 FT 1hr 5 FT 1hr

Uncond. 4hrs IDOT 4hrs 3 FT 4hrs 5 FT 4hrs

0

10

20

30

40

50

60

70

80

90

100

Control LAS LimeD SBS SBS+LAS PPA+LimeD RAP

TSR

(%

)

IL 1hr 3 FT 1hr 5 FT 1hr

IL 4hrs 3 FT 4hrs 5 FT 4hrs

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61

(a)

(b)

Figure 5.3 Complex modulus for control mixes: (a) 1 hr aging; (b) 4 hrs aging

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

Control 1h Dry

Control 1h IDOT

Control 1h 3 FT

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

Control 4h Dry

Control 4h IDOT

Control 4h 3FT

Control 4h 5FT

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(a)

(b)

Figure 5.4 Complex modulus for control mixes (a) 1 hr vs 4 hrs aging at unconditioned; (b) 1 hr

vs 4 hrs aging at IDOT conditioning

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

Control 1h Dry

Control 4h Dry

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

Control 1h IDOT

Control 4h IDOT

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63

(a)

(b)

Figure 5.5 Complex modulus for control mixes: (a) 1 hr vs 4 hrs aging at 3 FT; and (b) 1 hr vs 4

hrs aging at 5 FT

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

Control 1h 3 FT

Control 4h 3 FT

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

Control 1h 5 FT

Control 4h 5 FT

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64

(a)

(b)

Figure 5.6 Complex modulus for mixes with LAS: (a) 1 hr aging; (b) 4 hrs aging

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

LAS 1h DryLAS 1h IDOTLAS 1h 3FTLAS 1h 5FT

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

LAS 4h DryLAS 4h IDOTLAS 4h 3FTLAS 4h 5FT

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65

(a)

(b)

Figure 5.7 Complex modulus for mixes with LAS: (a) 1 hr vs 4 hrs aging at unconditioned; (b) 1

h vs 4 hrs aging at IDOT conditioning

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

LAS 1h Dry

LAS 4h Dry

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

LAS 1h IDOT

LAS 4h IDOT

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66

(a)

(b)

Figure 5.8 Complex modulus for mixes with LAS: (a) 1 h vs 4 hrs aging at 3 FT; and (b) 1 hr vs

4 hrs aging at 5 FT

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

LAS 1h 3 FT

LAS 4h 3 FT

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

LAS 1h 5 FT

LAS 4h 5 FT

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67

(a)

(b)

Figure 5.9 Complex modulus for mixes with LimeD: (a) 1 hr aging; (b) 4 hrs aging

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

LimeD 1h DryLimeD 1h IDOTLimeD 1h 3FTLimeD 1h 5FT

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

LimeD 4h DryLimeD 4h IDOTLimeD 4h 3FTLimeD 4h 5FT

Page 87: MECHANICAL AND SURFACE FREE ENERGY …

68

(a)

(b)

Figure 5.10 Complex modulus for mixes with LimeD: (c) 1 hr vs 4 hrs aging at unconditioned;

(d) 1 hr vs 4 hrs aging at IDOT conditioning

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

LimeD 1h Dry

LimeD 4h Dry

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

LimeD 1h IDOT

LimeD 4h IDOT

Page 88: MECHANICAL AND SURFACE FREE ENERGY …

69

(a)

(b)

Figure 5.11 Complex modulus for mixes with LimeD: (a) 1 hr vs 4 hrs aging at 3 FT; and (b) 1

hr vs 4 hrs aging at 5 FT

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

LimeD 1h 3 FT

LimeD 4h 3 FT

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

LimeD 1h 5 FT

LimeD 4h 5 FT

Page 89: MECHANICAL AND SURFACE FREE ENERGY …

70

(a)

(b)

Figure 5.12 Complex modulus for mixes with PPA+LimeD: (a) 1 hr aging; (b) 4 hrs aging

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

PPA+LimeD 1h Dry

PPA+LimeD 1h IDOT

PPA+LimeD 1h 3FT

PPA+LimeD 1h 5FT

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

PPA+LimeD 4h Dry

PPA+LimeD 4h IDOT

PPA+LimeD 4h 3FT

PPA+LimeD 4h 5FT

Page 90: MECHANICAL AND SURFACE FREE ENERGY …

71

(a)

(b)

Figure 5.13 Complex modulus for mixes with PPA+LimeD: (a) 1 hr vs 4 hrs aging at

unconditioned; (b) 1 hr vs 4 hrs aging at IDOT conditioning

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

PPA+LimeD 1h Dry

PPA+LimeD 4h Dry

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

PPA+LimeD 1h IDOT

PPA+LimeD 4h IDOT

Page 91: MECHANICAL AND SURFACE FREE ENERGY …

72

(a)

(b)

Figure 5.14 Complex modulus for mixes with PPA+LimeD: (a) 1 hr vs 4 hrs aging at 3 FT; and

(b) 1 hr vs 4 hrs aging at 5 FT

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

PPA+LimeD 1h 3 FT

PPA+LimeD 4h 3 FT

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

PPA+LimeD 1h 5 FT

PPA+LimeD 4h 5 FT

Page 92: MECHANICAL AND SURFACE FREE ENERGY …

73

(a)

(b)

Figure 5.15 Complex modulus for mixes with SBS: (a) 1 hr aging; (b) 4 hrs aging

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

SBS 1h Dry

SBS 1h IDOT

SBS 1h 3FT

SBS 1h 5FT

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

SBS 4h DrySBS 4h IDOTSBS 4h 3FTSBS 4h 5FT

Page 93: MECHANICAL AND SURFACE FREE ENERGY …

74

(a)

(b)

Figure 5.16 Complex modulus for mixes with SBS: (a) 1 hr vs 4 hrs aging at unconditioned; (b)

1 hr vs 4 hrs aging at IDOT conditioning

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

SBS 1h Dry

SBS 4h Dry

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

SBS 1h IDOT

SBS 4h IDOT

Page 94: MECHANICAL AND SURFACE FREE ENERGY …

75

(a)

(b)

Figure 5.17 Complex modulus for mixes with SBS: (a) 1 hr vs 4 hrs aging at 3 FT; and (b) 1 hr

vs 4 hrs aging at 5 FT

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

SBS 1h 3 FT

SBS 4h 3 FT

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

SBS 1h 5 FT

SBS 4h 5 FT

Page 95: MECHANICAL AND SURFACE FREE ENERGY …

76

(a)

(b)

Figure 5.18 Complex modulus for mixes with SBS+LAS: (a) 1 hr aging; (b) 4 hrs aging

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

SBS+LAS 1h Dry

SBS+LAS 1h IDOT

SBS+LAS 1h 3FT

SBS+LAS 1h 5FT

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

SBS+LAS 4h Dry

SBS+LAS 4h IDOT

SBS+LAS 4h 3FT

SBS+LAS 4h 5FT

Page 96: MECHANICAL AND SURFACE FREE ENERGY …

77

(a)

(b)

Figure 5.19 Complex modulus for mixes with SBS+LAS: (a) 1 hr vs 4 hrs aging at

unconditioned; (b) 1 hr vs 4 hrs aging at IDOT conditioning

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

SBS+LAS 1h Dry

SBS+LAS 4h Dry

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

SBS+LAS 1h IDOT

SBS+LAS 4h IDOT

Page 97: MECHANICAL AND SURFACE FREE ENERGY …

78

(a)

(b)

Figure 5.20 Complex modulus for mixes with SBS+LAS: (a) 1 hr vs 4 hrs aging at 3 FT; and (b)

1 hr vs 4 hrs aging at 5 FT

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

SBS+LAS 1h 3 FT

SBS+LAS 4h 3 FT

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

SBS+LAS 1h 5 FT

SBS+LAS 4h 5 FT

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79

(a)

(b)

Figure 5.21 Complex modulus for mixes with RAP: (a) 1 hr aging; (b) 4 hrs aging

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

RAP 1h DryRAP 1h IDOTRAP 1h 3FTRAP 1h 5FT

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

RAP 4h DryRAP 4h IDOTRAP 4h 3FTRAP 4h 5FT

Page 99: MECHANICAL AND SURFACE FREE ENERGY …

80

(a)

(b)

Figure 5.22 Complex modulus for mixes with RAP: (a) 1 hr vs 4 hrs aging at unconditioned; (b)

1 hr vs 4 hrs aging at IDOT conditioning

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

RAP 1h Dry

RAP 4h Dry

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

RAP 1h IDOT

RAP 4h IDOT

Page 100: MECHANICAL AND SURFACE FREE ENERGY …

81

(a)

(b)

Figure 5.23 Complex modulus for mixes with RAP: (a) 1 hr vs 4 hrs aging at 3 FT; and (b) 1 hr

vs 4 hrs aging at 5 FT

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

RAP 1h 3 FT

RAP 4h 3 FT

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

RAP 1h 5 FT

RAP 4h 5 FT

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82

Figure 5.24 Complex modulus for the mixes at 1 hr aging and unconditioned

Figure 5.25 Complex modulus for the mixes at 4 hrs aging and unconditioned

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

Control

LAS

LimeD

PPA+LimeD

SBS

SBS+LAS

RAP

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

Control

LAS

LimeD

PPA+LimeD

SBS

SBS+LAS

RAP

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83

Figure 5.26 Complex modulus for mixes at 1 hr aging and IDOT conditioning

Figure 5.27 Complex modulus for mixes at 4 hrs aging and IDOT conditioning

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

Control

LAS

LimeD

PPA+LimeD

SBS

SBS+LAS

RAP

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

Control

LAS

LimeD

PPA+LimeD

SBS

SBS+LAS

RAP

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84

Figure 5.28 Complex modulus for mixes at 1 hr aging and 3 FT conditioning

Figure 5.29 Complex modulus for mixes at 4 hrs aging and 3 FT conditioning

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

Control

LAS

LimeD

PPA+LimeD

SBS

SBS+LAS

RAP

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

Control

LAS

LimeD

PPA+LimeD

SBS

SBS+LAS

RAP

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85

Figure 5.30 Complex modulus for mixes at 1 hr aging and 5 FT conditioning

Figure 5.31 Complex modulus for mixes at 4 hrs aging and 5 FT conditioning

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

Control

LAS

LimeD

PPA+LimeD

SBS

SBS+LAS

RAP

15

150

1500

1.E-03 1.E-01 1.E+01 1.E+03

Mo

du

lus

(ksi

)

Reduced Frequency (Hz)

Control

LAS

LimeD

PPA+LimeD

SBS

SBS+LAS

RAP

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86

Table 5.1. Moisture Susceptibility Evaluation for N90 Control Mix

Set Tensile Strength

(psi)

TSR

(%)

N90 Control Unconditioned 61.1

81.9 Conditioned 50.1

Table 5.2 IDT Strength Results for Asphalt Mixes at Different Aging and Conditioning Periods

Mix

IDT 1 hr

Uncond.

(psi)

IDT 4 hrs

Uncond.

(psi)

IDT 1 hr

IDOT

(psi)

IDT 4 hrs

IDOT

(psi)

IDT 1 hr

3 FT

(psi)

IDT 4 hrs

3 FT

(psi)

IDT 1 hr

5 FT

(psi)

IDT 4 hrs

5 FT

(psi)

Control 61.0 73.7 50.0 64.8 36.5 46.5 27.6 33.4

LAS Mix 51.0 77.8 49.6 71.1 45.6 58.2 43.7 49.4

HL Mix 61.8 97.5 49.5 88.8 48.0 81.7 46.2 56.4

PPA+HL Mix 71.3 80.6 64.6 55.3 52.1 52.7 43.3 50.5

SBS Mix 75.4 86.8 74.0 82.4 60.3 62.5 45.2 51.4

SBS+LAS Mix 71.9 86.3 71.7 84.3 66.4 75.9 63.7 72.5

RAP Mix 117.8 125.7 102.9 106.2 90.7 79.5 78.8 67.6

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87

Table 5.3 TSR Values for Asphalt Mixes at Different Aging and Conditioning Periods

Mix TSR 1 hr-

IDOT (%)

TSR 4 hrs-

IDOT (%)

TSR 1 hr-

3 FT (%)

TSR 4 hrs-

3 FT (%)

TSR 1 hr-

5 FT (%)

TSR 4 hrs-

5 FT (%)

Control 82.0 88.0 59.8 63.1 45.2 45.2

LAS Mix 97.2 91.3 89.3 74.7 85.7 63.5

HL Mix 80.1 91.0 77.7 83.7 74.8 57.8

PPA+HL Mix 90.5 68.6 73.1 65.4 60.7 62.6

SBS Mix 98.1 94.9 80.0 72.0 59.9 59.2

SBS+LAS Mix 99.7 97.7 92.4 88.0 88.6 84.0

RAP Mix 87.4 84.5 77.0 63.3 66.9 53.8

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88

Table 5.4 Statistical Analysis for IDT (psi) of Control Mixes

Table 5.5 Statistical Analysis for IDT (psi) Tests of Mixes with LAS

Table 5.6 Statistical Analysis for IDT (psi) Tests of Mixes with LAS

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89

Table 5.7 Statistical Analysis for IDT (psi) Tests of Mixes with PPA+HL

Table 5.8 Statistical Analysis for IDT (psi) Tests of Mixes with SBS

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90

Table 5.9 Statistical Analysis for IDT (psi) Tests of Mixes with SBS+LAS

Table 5.10 Statistical Analysis for IDT (psi) Tests of Mixes with RAP

Table 5.11 Statistical Analysis for TSR (%) of Control Mixes

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91

Table 5.12 Statistical Analysis for TSR (%) of Mixes with LAS

Table 5.13 Statistical Analysis for TSR (%) of Mixes with HL

Table 5.14 Statistical Analysis for TSR (%) of Mixes with PPA+HL

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92

Table 5.15 Statistical Analysis for TSR (%) with Mixes with SBS

Table 5.16 Statistical Analysis for TSR (%) for Mixes with SBS+LAS

Table 5.17 Statistical Analysis for TSR (%) of Mixes with RAP

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93

CHAPTER 6 COMPONENT-LEVEL TESTS: RESULTS AND DISCUSSION

6.1 PREFACE

In this study, two aggregate, control binder, two additives, two modifiers, and a recycled

asphalt pavement (RAP) were used. The aggregate is dolomitic limestone and lime; the control

binder has a performance grade (PG) of 64-22; the additives are liquid anti-stripping (LAS) agent

and hydrated lime (HL); and the modifiers are polyphosphoric acid (PPA) and styrene butadiene

styrene (SBS). Seven asphalt binders were prepared from the control binder and selected

additives, modifiers and RAP: Control asphalt binder, Control+LAS asphalt binder, Control+HL

asphalt binder, Control+SBS (SBS) asphalt binder, Control+SBS+LAS (SBS+LAS) asphalt

binder, Control+PPA+HL (PPA+HL) asphalt binder, and Control+RAP asphalt binder.

In this study, three component-level tests were adopted to evaluate moisture susceptibility of the

aforementioned seven asphalt binders: surface free energy (SFE) test, direct adhesion test, and

blister test. The asphalt binder under component-level tests would be tested under virgin, RTFO

and PAV for status. The laboratory tests are presented in Chapter 4.

6.2 RESULTS AND DISCUSSION

6.2.1 Surface Free Energy

In this study, all asphalt binders tested were from the same source, share the same neat

asphalt binder PG64-22, and batched at the same time. Regarding aggregates, each type is

obtained from the same source and mined in the same day; aggregate source and sampling time

could have an impact on measured surface free energy.

Howson et al. 2009 studied the influence of source and sampling time on the surface energy of

asphalt binder and aggregate. For the same source, the measured surface free energy for asphalt

binder and aggregate is found to be batch dependent. However, the difference in aggregate

surface free energy did not alter their ranking. However, the ranking amongst asphalt binders

based on surface free energy had changed. This suggests that the surface free energy of asphalt

binder should be closely monitored and be measured more frequently.

In this study, a sessile drop device was used to measure the total SFE and SFE components for

the asphalt binder and aggregate. The sessile drop device is considered one of the most popular

and convenient methods for measuring SFE (Bahramian 2012, Koc and Bulut 2013, Lobato

2004, Wei and Zhang 2012). The sessile drop device measures SFE based on the contact angle

concept, which was first introduced in 1805 by Thomas Young (Zenkiewicz 2007). Determining

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94

the interaction energy between solids and liquids using contact angle is still considered one of

the most accurate methods (Lobato 2004, Zenkiewicz 2007).

It should be noted that the aggregate SFE measured by the sessile drop device is less than the

SFE measured using the universal sorption device because of the equilibrium spreading pressure

(Wei and Zhang 2012). Therefore, the compatibility energy ratios developed by Bhasin et al

2007a (ER1 and ER2) cannot be used. However, Wei and Zhang 2012 found the sessile drop

device capable of ranking aggregate based on their SFE.

The SFE for each of the adopted asphalt binders was measured at virgin, RTFO and PAV levels.

The purpose was to capture the effect of aging on the asphalt binder SFE and, consequently, the

effect of aging on both work of cohesion and work of adhesion. The total SFE energy, work of

adhesion, and work of cohesion will be calculated using Equations 10, 11, and 12, respectively,

in Chapter 4.

Seven asphalt binders and two aggregates were tested for their SFE. The asphalt binders are

control, control+LAS, control+HL, control+PPA+HL, control+SBS, control+SBS+LAS, and

control+RAP. The two aggregates are dolomitic limestone and lime. The seven asphalt binders

are of the same type used in the asphalt mixes. Dolomitic limestone is the source of CM11,

CM16, and FM20 while lime aggregate represents the source of HL.

A great number of studies have explored SFE as a tool for evaluating moisture damage.

However, this study contributes the following to the SFE field:

1. Using sessile drop device to evaluate the effect of aging (virgin vs RTFO vs PAV) on

asphalt binder total SFE, work of cohesion, and work of adhesion.

2. Using sessile drop device to evaluate the effect of HL, SBS, PPA+HL, and RAP on

asphalt binder total SFE, work of cohesion, and work of adhesion.

3. Using sessile drop device to measure the SFE of aggregate.

The RAP asphalt binder was extracted using the Rotary Evaporator. The extracted RAP asphalt

binder is called virgin RAP (Vr). The degree of oxidization that the RAP asphalt binder goes

through, starting from production throughout pavement service life, is unknown. Therefore,

several scenarios were prepared for each aging level based on the following two assumptions:

1. RAP asphalt binder undergoes short-term aging.

2. RAP asphalt binder does not undergo short-term aging.

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95

Based on the first assumption, Vr was aged by RTFO and was designated by (Rr). Then some of

the Rr was aged with PAV and designated by (PrwR). In the second assumption, some of the Vr

was immediately aged using PAV and designated by (PrnoR). For the purpose of simplification,

virgin, RTFO, and PAV control asphalt binder was designated by Vc, Rc, and Pc, respectively.

The following are the scenarios prepared to represent all aging levels for the RAP asphalt mix:

1. Virgin

a. Vc+Vr.

2. RTFO

a. Rc+Vr

b. Rc+Rr

3. PAV

a. Pc+PrnoR

b. Pc+PrwR

Despite the aging level, the amount of control and RAP asphalt binders added together was

proportional to the RAP asphalt mix design.

Preparing samples with HL is something that has never been done before in a study considering

SFE. HL was added to control and PPA-modified asphalt binders to produce Control+HL and

PPA+HL samples, respectively. The amount of HL added to control and PPA- modified asphalt

binders was proportional to the Control+HL and PPA+HL mix designs, respectively. The

preparation of SFE samples with HL requires heating the binder (virgin or RTFO or PAV)

enough to be in a workable status before adding the designated quantity of HL. Careful attention

should be given to mixing of HL with the asphalt binder to ensure homogeneity of the final

product. The asphalt binder-HL mixture was then poured in the SFE energy molds shown in

Figure 4.3.

In this study, three probe liquids were used. For each probe liquid, the contact angle was

measured with the surface of either asphalt binder or aggregate. The three liquids are water,

glycerol, and diiodomethane. When choosing probe liquids, at least three liquids must be chosen

and one of the three should be nonpolar (acid component = base component = 0) (Zenkiewicz

2007). In this case, diiodomethane is the nonpolar liquid while water and glycerol are the polar

liquids. The total SFE and SFE components of the adopted probe liquids are shown in Table A.1

in APPENDIX A.

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96

The contact angles measured for each asphalt binder with the probe liquids at each aging level

are shown in APPENDIX A (Table A.2 to Table A.8). The contact angles measured for the

aggregate with the probe liquids are shown in APPENDIX A (Table A.9). Based on the

measured contact angles, all results shown in Table 6.1 to Table 6.7 were calculated. Figure 6.1

and Figure 6.2 are the graphical representation of the results listed in Table 6.1, Table 6.2 and

Table 6.3, while Figure 6.3 is the graphical representation of the results shown in Table 6.5, to

Table 6.7.

Table 6.1 to Table 6.3 show the total SFE, SFE components, and work of cohesion for asphalt

binders at virgin, RTFO, PAV, respectively. Table 6.5 to Table 6.7 show the work of adhesion of

asphalt binders with dolomitic limestone at virgin, RTFO, and PAV, respectively.

The total SFE and SFE components of asphalt binders displayed in Table 6.1 to Table 6.3 agree

with the typical magnitude of SFE components developed by Little and Bhasin 2006. Little and

Bhasin 2006 reported that the typical magnitude of SFE components is as follows:

1. Total SFE: 15 to 45 energy/cm2.

2. LW component: Varies based on the type of asphalt binder and has the major impact on

total SFE of asphalt binder.

3. Acid-base components: in case the asphalt is basic as in this case, the acid component is

very close to zero while the basic component is higher. The values of acid and base

components will be reversed in case asphalt binder is acidic.

Because the acid components of the asphalt binders and aggregate in this study are small, the

LW and basic components had the major contribution to both works of adhesion and cohesion,

based on Equations 11 and 12.

Moisture damage occurs at the early stages of the pavement service life (Hicks 1991), meaning

that the asphalt binder will have undergone at least the short-term aging (production through

construction period). Thus, measuring SFE virgin (unaged) asphalt binder is impractical.

However, measuring the SFE for unaged asphalt binder gives an idea about the influence of

aging (RTFO and PAV) on SFE.

The data presented in Table 6.4 are consistent with the findings of other studies which indicate

that aggregate has a higher SFE compared with asphalt binder, and that aggregate has a

significantly higher base component compared with its acid component (Bhasin et al. 2006,

Little and Bhasin 2006, Masad et al. 2006b).

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97

At the virgin level (Table 6.1 and Figure 6.1), LAS additive and RAP asphalt binder showed

better SFE compared with the control asphalt binder. Therefore, control+LAS, SBS+LAS, and

Vc+Vr all produced the highest SFE and almost to the same level. On the other hand, adding HL

to the control asphalt binder and PPA-modified asphalt binder had almost no effect when

compared with the control asphalt binder. The same observation was made for the SBS-modified

asphalt binder. Thus, the immediate positive influence of LAS was observed on the increase of

SFE whether added to unmodified (control asphalt binder) or modified (SBS asphalt binder)

asphalt binders. The influence of HL is not obvious at the virgin level. Although both LAS and

HL were used to increase moisture resistance, LAS showed an improvement, unlike HL.

However, conclusions cannot be drawn at this level because moisture damage exists after the

short-term aging of asphalt mixes.

At the RTFO level (Table 6.2 and Figure 6.1), LAS and RAP asphalt binder improved the SFE in

comparison with the control asphalt binder. The impact of HL was obvious at this aging level as

a significant improvement of SFE was noted when HL was added to the control asphalt binder.

However, this improvement was not observed when HL was added to the PPA-modified asphalt

binder. In fact, the SFE of control, PPA+HL, and SBS asphalt binders showed almost no change

as a result of aging.

The highest SFE at RTFO resulted from the addition of RAP. There was no significant difference

between the Rc+Vr and Rc+Rr, thus implying RAP aging under RTFO does not alter its

properties. In addition, the SFE of Rc+Vr and Rc+Rr almost had a similar SFE to Vc+Vr. There

was not any changes in SFE as a result of aging in the case of RAP.

Although LAS improved the SFE of control and SBS-modified asphalt binders, there was a

reduction in SFE compared with the virgin state. This is a clear indication that the influence of

LAS reduces with aging. On the other hand, HL seems to improve SFE with aging.

Compared with the RTFO aged and the virgin binder, the SBS-modified asphalt binder and

control asphalt binder did not significantly change under PAV aging (Table 6.3 and Figure 6.1).

It was noted that the SBS-modifier asphalt binder may increase the stiffness of asphalt binder but

it has no effect on SFE. Further reduction is observed in SFE for control+LAS with aging. After

PAV control+LAS had almost the same SFE as for control asphalt binder. This indicates that the

influence of LAS diminishes with aging. However, SBS+LAS after PAV maintained the same

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SFE as after RTFO aging. This means that the addition of LAS improves the performance of

modified asphalt binders better than the unmodified asphalt binders with regard to SFE.

On the other hand, HL improved SFE with aging. Control+HL after PAV had the same SFE

value as after RTFO aging, while PPA+HL improved significantly after PAV. PAV aging

reduced SFE in the case of RAP (Pc+PrnoR and Pc+PrwR). No significant differences were

observed between the two PAV aging for RAP (Pc+PrnoR and Pc+PrwR).

In general, asphalt binders can be categorized into three categories based on the effect of aging

on SFE: SFE not effected by aging, such as control and SBS-modified asphalt binders; SFE

decreasing with aging, such as control+LAS, SBS+LAS, and RAP; and SFE increasing with

aging, such as control+HL and PPA+HL.

The SFE of lime aggregate (the source of HL used in this study) is higher compared with that of

dolomitic limestone, as seen in Table 6.4. This finding agrees with the results obtained from the

modified AASHTO and SFE tests. HL increased moisture resistance and SFE when added to the

asphalt mix and asphalt binder, respectively. The aggregate SFE findings contributes to the

ability of the sessile drop device to distinguish and rank aggregates based on their SFE. It should

be noted that for the work of adhesion, only the SFE of dolomitic limestone is used because the

lime aggregate is represented by HL that is already added to asphalt binder.

The work of cohesion is proportional to the SFE of asphalt binder, as shown in Figure 6.2. The

higher the SFE, the higher the work of cohesion. The work of cohesion had the same trend as the

SFE of asphalt binders. Therefore, the work of cohesion did not change with aging in the control

and SBS-modified asphalt binders; decreased with aging in control+LAS, SBS+LAS, and RAP;

and increased with aging in control+HL and PPA+HL.

The same observation was made for the work of adhesion, as shown in Figure 6.3. The higher the

SFE of asphalt binder and aggregate, the higher the work of adhesion. In this study, the work of

adhesion was calculated between dolomitic limestone and each of the seven asphalt binders.

Thus, any change in work of adhesion is related to the SFE of asphalt binders. Therefore, the

work of adhesion followed the trends of the SFE of asphalt binder. In other words, the work of

adhesion did not significantly change with aging for control and SBS-modified asphalt binders

because their SFE was not influenced by aging. The work of adhesion decreased with aging for

control+LAS, SBS+LAS, and RAP because their SFE decreased with aging. And, finally, the

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work of adhesion increased with aging for control+HL and PPA+HL because their SFE

increased with aging.

An interesting finding is observed for the work of adhesion between control asphalt binder at

PAV with dolomitic limestone which was significantly high compared with the work of adhesion

at RTFO. The control asphalt binder had almost the same SFE at RTFO and PAV. However,

looking at the SFE components, the control asphalt binder at PAV had a higher base component

compared with RTFO and virgin. The increase in the base component at PAV for the control

asphalt binder was sufficient to boost the work of adhesion compared with the RTFO and virgin

states. However, both LAS and the control ended having almost the same work of adhesion.

Again, this shows that the LAS influence on SFE and adhesion diminishes with aging.

It is important to consider SFE components carefully when studying the works of adhesion and

cohesion. The higher the work of adhesion and work of cohesion, the higher the resistance to

adhesion and cohesion failures, respectively. Therefore, the following findings are drawn:

1. LAS and HL improved moisture resistance because both had increased work of adhesion

and cohesion. However, the impact of LAS decreased with aging while that of HL

increased. The impact of LAS and HL was observed in spite of the fact that they were

added to unmodified asphalt binder (control) and modified asphalt binder (SBS-modified

and PPA-modified). However, the modified asphalt binder with LAS, such as SBS+LAS,

seems to have better resistance to aging (SBS+LAS SFE at RTFO almost same as

SBS+LAS SFE at PAV).

2. Control+LAS at PAV almost had the same SFE, work of adhesion, and cohesion for the

control asphalt binder.

3. RAP improved moisture resistance because both had increased work of adhesion and

cohesion. The influence of RAP decreased with aging. The scenarios prepared with RAP

at RTFO and PAV had no significant difference in performance.

4. The SFE of control and SBS-modified asphalt binders, work of adhesion and cohesion

almost did not alter with aging. This was not the case for control asphalt binder at PAV

where its high base component resulted in higher work of adhesion compared with RTFO

and virgin levels.

5. Work of adhesion and cohesion follow the same trend as SFE. The higher the SFE, the

higher the work of adhesion and cohesion and vice versa.

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Adding HL to control and PPA-modified asphalt binders improved moisture resistance. The

positive impact of HL increased with aging. Thus, the highest SFE, and work of adhesion and

cohesion were noticed after PAV aging. However, the impact of HL in case PPA+HL asphalt

binder was triggered after PAV aging and after RTFO aging for control+HL. This could be

explained by the fact that PPA reduces the aging rate, which may therefore delay the impact of

HL until after PAV aging, whereas PPA is not as efficient in RTFO aging.

It is reported in the literature that HL and LAS are the two most common additives used to

mitigate moisture damage in asphalt mixtures (Souliman et al. 2014). It is also reported that both

perform well at the early stages of pavements service life with preferences sometimes for HL or

LAS (Hao and Hachiya 2003; Kennedy and Ping 1991; Kennedy and Roberts 1982; Little and

Petersen 2005; Maupin Jr. 1995; Sebaaly 2007b; Stroup-Gardiner and Epps 1990). However, it is

known that HL demonstrates a better performance with long-term aging (late pavement service

life) (Hicks and Scholz 2001; Khosla and Harikrishnan 2007; Lesueur and Little 1999; Little and

Epps 2011; Mohammad et al. 2000; Petersen et al. 1987, Souliman et al. 2014; Tayebali, 2003;

Zaniewski and Viswanathan 2006). These literature findings are in agreement with the

observations made with regard to SFE for LAS and HL. The SFE test shows that both LAS and

HL improve performance against moisture and that HL has a better long-term performance

compared with LAS. The fact that the sessile drop device was able to capture these trends in the

component scale reflects the efficiency of this device and its ability to evaluate different asphalt

binders with different additives at various aging levels.

Mohammad and Morshed 2008 studied the impact of aging on the physical and chemical

properties of asphalt binder and observed that asphaltenes compound content increases with

aging. The increase in asphaltenes content reduces the adhesion properties in asphalt binder

(Buckley and Morrow 1991). The increasing rate of asphaltenes with aging is slower for HL-

modified asphalt binder compared with HL-free asphalt binders (Hopman 1998; Petersen et al.

1987; Plancher et al. 1976; Verhasselt and Puiatti 2004; Wisneski et al. 1996). This is why the

HL-modified asphalt binder shows a reduced effect of aging (slower asphaltenes increase rate)

which happens because the polar particles in asphalt binder are adsorbed and neutralized by the

HL particles (Petersen et al. 1987; Plancher et al. 1976; Sebaaly 2006). This neutralization

prevents further chemical aging in asphalt binder. Overall, this explains the significant

improvement of SFE when adding HL.

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Lesueur and Little (1999) reported that HL needs several hours of heating for its effect to build-

up. Control+HL and PPA+HL share the same HL content. In the control+HL mix, the HL effect

was noticed after RTFO aging; prolonged PAV aging was needed before the effect of HL was

observed in PPA+HL due to the fact that PPA reduces aging. Thus, it would not be possible to

observe the effect of HL on asphalt mixes if the heating process is not sufficient (Lesueur and

Little 1999). Therefore, LAS has an instant impact on asphalt mixes while HL requires additional

aging and heat to have an influence on asphalt mixes.

Typically, LAS contains amines compound (Tunnicliff and Root 1983; Wasiuddin et al. 2007b).

The amines compound interacts with the asphaltenes in asphalt binder, which enhances the

adhesion properties of asphalt binder, thus increasing SFE. Although in this study the LAS

improved the performance of asphalt binder, this is not always the case. Western Research

Institute (2006) reported that liquid antistrips possess different efficiencies when added to

different asphalt binders.

LAS undergoes thermal degradation as a result of aging, heating, and storage (Dybalski 1982;

Tarrer and Wagh 1991). The thermal degradation of LAS reduces the concentration of LAS

(Bagampadde 2005; Yoon et al. 1993) and, consequently, its effectiveness as in improving the

adhesion performance of asphalt binder. Wasiuddin et al. 2007b found that the impact of aging

and thermal degradation is higher on PG 64-22 than modified binders, such as the case in this

study (control+LAS vs SBS+LAS).

The addition of RAP to asphalt mixes improves their moisture resistance (Tiwari and Patel 2014;

Zhou et al. 2011). Aurangzeb et al. 2012 found that moisture susceptibility decreases with the

increase in RAP content in asphalt mixes. A performance improvement was noticed in this study

when RAP asphalt binder was added to the control binder by increasing the SFE, thereby

improving the adhesion with aggregate. Aging reduced the SFE of control asphalt binder with

RAP. This might be attributed to the increase of asphaltenes compound with aging, thus reducing

the adhesion performance of asphalt binder (Buckley and Morrow 1991).

Results from the SFE test suggest that there is no unique relation between SFE parameters (SFE,

work of adhesion, and work of cohesion) and aging. SFE parameters may increase, decrease, or

remain unchanged with aging. The literature reports that the aging impact is dependent on the

initial chemistry and rheology of the unaged asphalt binder and added polymers (Lu and Isacsson

2000; Western Research Institute 2006; Howson et al. 2007). The oxidation reaction kinetics

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occurring while aging and the duration of aging may also affect the relation between SFE and

aging (Howson et al. 2007).

Howson et al. 2007 used the Wilhelmy plate method to test different asphalt binders with several

additives and modifiers under different aging periods. Changes were observed in SFE

components, but no general trend was noticed. It was speculated that the changes in the polar

groups of unaged asphalt binder resulted in changes in the surface properties of aged asphalt

binders. The SFE for each asphalt binder should be measured to recognize the relation between

SFE parameters and aging.

6.2.2 Direct Adhesion Test

Table 6.8 displays the Pmax and bond energy (E) values for all asphalt binders. Figure 6.4 and

Figure 6.5 represents the graphical results of Pmax and E, respectively. Results from Figure 6.4

and

Figure 6.5 are summarized in the following bullets:

1. Virgin - Pmax:

a. LAS-modified asphalt binder had the highest Pmax while RAP produced the lowest

Pmax.

b. LAS significantly increased Pmax with respect to Control asphalt binder.

c. RAP and PPA+HL significantly reduced Pmax with respect to Control asphalt

binder.

d. Control+HL, SBS, and SBS+LAS had no significant influence on Pmax with

respect to Control asphalt binder.

2. RTFO - Pmax:

a. LAS-modified asphalt binder had the highest Pmax while RAP produced the lowest

Pmax.

b. LAS, SBS, SBS+LAS, Control+HL and PPA+HL significantly increased Pmax

with respect to Control asphalt binder.

c. RAP significantly reduced Pmax with respect to Control asphalt binder.

3. Virgin - E:

a. LAS-modified asphalt binder had the highest E while RAP produced the lowest E.

b. LAS and SBS+LAS significantly increased E with respect to Control asphalt

binder.

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c. Control+HL, PPA+HL, and RAP significantly reduced E with respect to Control

asphalt binder.

d. SBS had no significant influence on E with respect to Control asphalt binder.

4. RTFO - E:

a. LAS and SBS significantly increased E with respect to Control asphalt binder.

b. RAP significantly reduced E with respect to Control asphalt binder.

c. Control+HL, PPA+HL, and SBS+LAS had no significant influence on E with

respect to Control asphalt binder.

5. Except for Control and SBS+LAS asphalt binders, there was no significant difference

when comparing Pmax at virgin with RTFO for each asphalt binder. In case of E (bond

energy), there was no significant difference when comparing virgin with RTFO except

for Control, SBS+LAS and RAP asphalt binders.

Generally, LAS had the best adhesion properties when added to Control and SBS-modified

asphalt binders. On the other hand, RAP had the least adhesion amongst all asphalt binders. The

influence of HL was not following a certain trend compared to control asphalt binder. The

influence of SBS ranged from no significant alteration to significant increase in adhesion

properties with respect to Control, SBA+LAS asphalt binder.

The improved adhesion properties resulting from the addition of LAS is in agreement with the

findings of SFE test. However, DAT and SFE show completely contradicting results when it

comes to the influence of RAP and HL. In addition, DAT differs from SFE in its inability to

capture the impact of aging on adhesion properties for the considered asphalt binders in this

study, except for the Control and SBS+LAS asphalt binders and also RAP in one case.

Another research team working on crack sealants at the Illinois Center for Transportation (ICT)

conducted extensive testing using DAT to determine the adhesion properties for several types of

crack sealants. They found that this test is not reliable enough to rank and classify different crack

sealants based on their adhesion properties. The following major drawbacks were found

considering DAT test procedure and results:

1. Sample preparation: The results of DAT vary from one operator to the other. Sample

preparation requires trimming the excess asphalt binder, removing the shim, and

removing the bottom aluminum base (see Figure 6.6 to Figure 6.8); any mistake could

disturb the sample and affect the results.

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2. Repeatability: Table 6.9 displays the coefficient of variance (COV) for Pmax and E at

virgin and RTFO state. COV is relatively high for most asphalt binders. Many samples (≥

6) for each asphalt binder were tested to get repeatable results.

3. Sample failure: In DAT, the sample should fail perpendicular to the cross section.

However, several samples failed in a tilting manner (see Figure 6.9), which will definitely

affect the measured results due to bending.

In conclusion, Pmax and E are two parameters measured and calculated from the DAT test to

evaluate and predict adhesion. It was noticed that DAT is not an appropriate qualitative method

for evaluating the adhesion properties of asphalt binder. Currently, due to the aforementioned

DAT test drawbacks, a research group at ICT is working on developing a new adhesion test able

to produce more repeatable and reliable results. Thus, no solid conclusions are drawn from the

current DAT test.

6.2.3 Blister Test

The blister test (BT) was originally developed to evaluate the interfacial adhesion

properties of crack sealants. In this study, BT was applied on asphalt binders. The main criteria

for a successful BT is the occurrence of blister along with full separation between the asphalt

binder and the aluminum substrate.

The asphalt binders tested in this study are the same tested using DAT. Using standard samples

(see Figure 4-8), all asphalt binders failed the BT test. In other words, no separation occurred

between any of the tested asphalt binder and aluminum substrate. The research team then

decided to try BT samples with different dimensions (thickness, diameter, and orifice diameter)

tested under different temperatures (> 4°C) and loading rates (0.1L/h and 1 L/h), as seen in

Figure 6.10 to Figure 6.12. Despite any combination (thickness, diameter, orifice diameter,

temperature, and loading rate), all samples failed to show any separation, see Figure 6.13 to

Figure 6.16.

Based on this, BT with current setup is concluded to be an unsuitable for evaluating the adhesion

properties of asphalt binder.

6.3 SUMMARY

In this chapter, the components of the asphalt mixes tested in chapter 5 were tested using

three component-level tests, namely; surface free energy (SFE) test, direct adhesion test, and

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blister test. The SFE results show that the sessile drop device is an efficient tool to evaluate

different asphalt binders with different additives at various aging levels.

SFE results show that aggregate had higher SFE than asphalt binder. It was found that LAS, HL

and RAP produced the best performance considering moisture resistance when added to asphalt

binder. LAS and HL enhanced unmodified or modified asphalt binder. However, LAS and RAP

improvement decreased with aging while HL improvement increased with aging. PPA and SBS

modifiers produced insignificant alteration of control asphalt binder SFE. Results from the SFE

test suggest that there is no unique relation between SFE parameters (SFE, work of adhesion, and

work of cohesion) and aging since it is dependent on the initial chemistry and rheology of the

unaged asphalt binder and added polymers.

The DAT outcomes showed that LAS and RAP had the best and least adhesion performance,

respectively. DAT and SFE results are completely contradictory considering the influence of

RAP, HL, SBS and PPA. DAT appears to be incapable of capturing aging impact on adhesion

performance (either increasing or decreasing) and unreliable in ranking and classifying asphalt

binders. This could be related to the drawbacks in sample preparation, repeatability, and sample

failure.

The current BT setup needs improvement to be able to properly assess the adhesion

characteristics of asphalt binder.

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Chapter 6 Figures and Tables

Figure 6.1 SFE of asphalt binder at the virgin, RTFO, and PAV aging levels.

Figure 6.2 Work of cohesion of asphalt binder at the virgin, RTFO, and PAV aging levels.

0.0

5.0

10.0

15.0

20.0

25.0

30.0

35.0

40.0

Control Control+LAS Control+HL PPA+HL SBS SBS+LAS RAP

SFE

(en

ergy

/cm

2)

Virgin RTFO PAVRc+Vr

Pc+PrnoRRc+Rr

Pc+PrwR

0.0

10.0

20.0

30.0

40.0

50.0

60.0

70.0

80.0

90.0

Control Control+LAS Control+HL PPA+HL SBS SBS+LAS RAP

Wo

rk o

f C

oh

esio

n (

ener

gy/c

m2)

Virgin RTFO PAV Rc+VrRc+Rr

Pc+PrnoR Pc+PrwR

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107

Figure 6.3 Work of adhesion of asphalt binder with dolomitic limestone at the virgin, RTFO, and

PAV aging levels.

Figure 6.4 Peak load (Pmax) for asphalt binders at virgin and RTFO state.

75.0

80.0

85.0

90.0

95.0

100.0

105.0

Control Control+LAS Control+HL PPA+HL SBS SBS+LAS RAP

Wo

rk o

f A

dh

esio

n (

ener

gy/c

m2)

Virgin RTFO PAVRc+Vr

Pc+PrnoR

Rc+Rr

Pc+PrwR

0.0

10.0

20.0

30.0

40.0

50.0

Control Control+LAS Control+HL PPA+HL SBS SBS+LAS RAP

Pm

ax (

N)

Peak Load - Pmax

Virgin

RTFO

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Figure 6.5 Bond energy (E) for asphalt binders at virgin and RTFO state.

Figure 6.6 Trimming the DAT sample excessive asphalt binder.

0.0

2.0

4.0

6.0

8.0

10.0

Control Control+LAS Control+HL PPA+HL SBS SBS+LAS RAP

Bo

nd

En

ergy

(J/

m2)

Bond Energy - E

Virgin

RTFO

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Figure 6.7 Removing the shim from DAT sample prior to testing.

Figure 6.8 Removing the DAT sample bottom aluminum base.

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Figure 6.9 Tilting failure.

Figure 6.10 BT sample with smaller diameter.

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Figure 6.11 BT sample with original diameter and half-original thickness.

Figure 6.12 BT sample with original diameter and double original thickness.

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Figure 6.13 No separation for BT sample with smaller diameter.

Figure 6.14 No separation for BT sample with original diameter and half-original thickness.

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Figure 6.15 No separation for BT sample with original diameter, double original thickness, and

small orifice diameter.

Figure 6.16 No separation for BT sample with original diameter, double original thickness, and

large orifice diameter.

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Table 6.1 SFE for Asphalt Binder and Work of Cohesion at the Virgin Level

Virgin

Binder

Total

(energy/cm2)

LW

(energy/cm2)

Acid

(energy/cm2)

Base

(energy/cm2)

Work of Cohesion

(energy/cm2)

Control 32.5 31.6 0.1 2.1 65.0

Control+LAS 38.9 29.7 1.4 15.5 77.7

Control+HL 32.8 30.2 0.4 3.8 65.6

PPA+HL 32.2 30.0 0.4 3.6 64.5

SBS 32.1 30.4 0.2 3.4 64.2

SBS+LAS 37.9 29.9 1.3 12.2 75.8

Vc+Vr* 38.6 33.5 0.7 8.9 77.3

*Virgin control asphalt binder + Virgin (Extracted) RAP asphalt binder

Table 6.2 SFE for Asphalt Binder and Work of Cohesion at the RTFO Level

RTFO Binder Total

(energy/cm2)

LW

(energy/cm2)

Acid

(energy/cm2)

Base

(energy/cm2)

Work of Cohesion

(energy/cm2)

Control 33.0 32.1 0.1 1.6 66.1

Control+LAS 36.1 31.1 0.8 7.4 72.2

Control+HL 36.1 33.2 0.6 3.5 72.3

PPA+HL 32.9 31.3 0.2 2.5 65.8

SBS 31.4 29.7 0.3 2.6 62.7

SBS+LAS 34.3 31.7 0.5 3.1 68.5

Rc+Vr* 39.1 35.0 0.7 6.4 78.2

Rc+Rr** 38.0 33.7 0.6 7.7 76.1

*RTFO control asphalt binder + Virgin (Extracted) RAP asphalt binder

**RTFO control asphalt binder + RTFO RAP asphalt binder

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115

Table 6.3 SFE for Asphalt Binder and Work of Cohesion at the PAV Level

PAV Binder Total

(energy/cm2)

LW

(energy/cm2)

Acid

(energy/cm2)

Base

(energy/cm2)

Work of Cohesion

(energy/cm2)

Control 33.6 30.1 0.5 6.5 67.3

Control+LAS 33.3 30.8 0.4 4.5 66.7

Control+HL 36.1 33.1 0.7 3.3 72.1

PPA+HL 37.9 33.2 1.0 5.5 75.7

SBS 31.4 29.7 0.3 2.8 62.7

SBS+LAS 34.5 31.4 0.6 4.1 69.0

Pc+PrnoR* 35.7 32.4 0.6 4.7 71.4

Pc+PrwR** 34.9 31.8 0.5 5.1 69.9

*PAV control asphalt binder + PAV RAP asphalt binder without RTFO

**PAV control asphalt binder + PAV RAP asphalt binder with RTFO

Table 6.4 SFE for aggregate

Aggregate Total

(energy/cm2)

LW

(energy/cm2)

Acid

(energy/cm2)

Base

(energy/cm2)

Dolomitic Limestone 63.2 47.0 1.4 45.6

Lime 80.1 49.4 4.5 52.7

Table 6.5 Work of Adhesion of Asphalt Binder with Dolomitic Limestone at the Virgin Level

Virgin Work of Adhesion with Dolomitic Limestone

(energy/cm2)

Control 84.9

Control+LAS 99.9

Control+HL 89.0

PPA+HL 87.7

SBS 86.3

SBS+LAS 98.8

Vc+Vr 98.1

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116

Table 6.6 Work of Adhesion of Asphalt Binder with Dolomitic Limestone at the RTFO Level

RTFO Work of Adhesion with Dolomitic Limestone

(energy/cm2)

Control 85.7

Control+LAS 95.3

Control+HL 94.2

PPA+HL 87.2

SBS 85.5

SBS+LAS 91.3

Rc+Vr 98.1

Rc+Rr 96.8

Table 6.7 Work of Adhesion of Asphalt Binder with Dolomitic Limestone at the PAV Level

PAV Work of Adhesion with Dolomitic Limestone

(energy/cm2)

Control 90.7

Control+LAS 89.4

Control+HL 94.2

PPA+HL 98.0

SBS 85.5

SBS+LAS 92.1

Pc+PrnoR 93.4

Pc+PrwR 92.1

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Table 6.8 Pmax and E for Asphalt Binders at Virgin and RTFO State

Binder Virgin RTFO

Pmax (N) E (J/m2) Pmax (N) E (J/m2)

Control 29.1 4.86 16.1 2.04

Control+LAS 40.8 8.06 39.7 7.00

Control+HL 24.8 2.79 21.6 1.76

PPA+HL 21.2 2.09 19.4 1.49

SBS 24.7 5.02 32.7 5.33

SBS+LAS 27.9 6.87 24.7 2.0

RAP 11.9 1.88 7.4 0.45

Table 6.9 Coefficient of Variance (in Percent) for Pmax and E at Virgin and RTFO State

Binder

Virgin RTFO

Pmax

(N)

COV

E (J/m2)

COV

Pmax

(N)

COV

E (J/m2)

COV

Control 37.9 39.40 23.2 43.3

Control+LAS 11.7 11.84 12.4 29.8

Control+HL 17.9 36.08 18.7 31.9

PPA+HL 12.9 23.98 8.0 22.6

SBS 48.5 83.84 19.9 8.7

SBS+LAS 9.3 19.81 4.5 54.8

RAP 25.8 40.13 51.2 77.8

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CHAPTER 7 MIXTURE AND COMPONENT LEVEL RELATIONSHIP

7.1 INTRODUCTION

In Chapters 5 and 6, the results of the mixture- and component-level tests were displayed

and discussed, respectively. The mixture-level test consists of the modified Lottman test

(AASHTO T-283) and dynamic modulus test (AASHTO T 342). The two tests were conducted

on seven asphalt mixes: Control, Control+LAS, Control+HL, PPA-modified+HL, SBS-modified,

SBS-modified+LAS, and 50% RAP mix.

On the other hand, three component-level tests were adopted: SFE, DAT and blister test. The

component tests were applied on seven asphalt binders (Control, Control+LAS, Control+HL,

PPA-modified+HL, SBS-modified, SBS-modified+LAS, and RAP asphalt binders) and two

types of aggregate (dolomitic limestone and lime).

The objective was to study the correlation, similarities, and differences, if any, between the

component- and mixture-level tests as well as within the mixture-level tests themselves. In this

chapter, only the two mixture-level tests and SFE are considered.

7.2 DYNAMIC MODULUS RATIO

It is not practical or possible to compare master curves from the dynamic modulus test

with TSR and total SFE values from the modified Lottman and SFE tests, respectively. Master

curves indicate the material performance over a wide spectrum of temperatures and frequencies.

Thus, a specific value should be identified from the dynamic modulus test to simplify the

comparison.

In this study, the approach suggested by Nadkarni et al. (2009) to develop a specific value from

the dynamic modulus test was adopted. Nadkarni et al. (2009) proposed a dynamic modulus ratio

(E* Ratio) at each of the six frequencies (25, 10, 5, 1, 0.5, and 0.1 Hz) at 21°C. The E* Ratio

was proposed to evaluate asphalt mixture moisture damage. The E* Ratio is the relative relation

of dynamic modulus after conditioning (IDOT, 3 FT, or 5 FT) to dynamic modulus prior to

conditioning (unconditioned). The final reported E* Ratio is the average of the six E* Ratios.

Table 7.1(a) and (b) display an E* Ratio sample calculation for Control asphalt mixture after 1 hr

short-term aging. Similarly, E* Ratio was calculated for all asphalt mixes after 1 hr and 4 hrs

short-term aging, as shown in Table 7.2 and Table 7.3 and, respectively. APPENDIX B displays

all E* Ratio calculations for all asphalt mixes.

Therefore, the E* Ratio in Table 7.2 and Table 7.3 was used to compare with TSR and total SFE.

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7.3 MODIFIED AASHTO VS. DYNAMIC MODULUS

For the comparison to be reliable, a statistical analysis was conducted using SPSS to

check the extent of variation in the performance of the asphalt mixes. The statistical analysis was

done for both TSR and E* Ratio parameters. Six cases were identified for each parameter

wherefore the analysis was conducted: 1 hr short-term aging with IDOT conditioning, 1 hr short-

term aging with 3 FT conditioning, 1 hr short-term aging with 5 FT conditioning, 4 hrs short-

term aging with IDOT conditioning, 4 hrs short-term aging with 3 FT conditioning, and 4 hrs

short-term aging with 5 FT conditioning.

Table 7.4 to Table 7.9 display the six cases for E* Ratio. Table 7.10 and Table 7.11 show the

TSR results for asphalt mixes after 1 hr and 4 hrs short-term aging respectively. The six cases for

TSR are displayed from Table 7.12 to Table 7.17.

The following comparison will be focusing on comparing the E* Ratio outcome with TSR

outcome at each case and not vice versa. In other words, the outcome of TSR is the reference.

This is because TSR is already the widely used tool for evaluating moisture susceptibility of

asphalt mixtures.

7.3.1 1 hr short-term aging and IDOT conditioning

E* Ratio, Table 7.4:

Asphalt mixes showed no significant impact on moisture resistance compared with

Control asphalt mix, except for RAP, HL, and SBS+LAS

RAP resulted in significant reduction while HL (Control+HL) and SBS+LAS improved

moisture resistance compared with Control asphalt mix

TSR, Table 7.12:

Additives/modifiers had improved moisture resistance compared with Control asphalt

mix, except for HL (Control+HL) and RAP

Control+HL and RAP showed no significant impact on moisture resistance compared

with Control asphalt mix

7.3.2 1 hr short-term aging and 3 FT conditioning

E* Ratio, see Table 7.5:

Asphalt mixes showed no significant impact on moisture resistance, except for RAP,

Control+HL, and SBS+LAS, compared with Control asphalt mix

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RAP and SBS+LAS resulted in significant reduction in performance while Control+HL

significantly improved performance compared with Control mix

TSR, Table 7.13:

Asphalt mixes showed moisture resistance improved significantly compared with Control

asphalt mix, with preference to LAS (SBS+LAS and Control+LAS)

7.3.3 1 hr short-term aging and 5 FT conditioning

E* Ratio, Table 7.6:

LAS (SBS+LAS and Control+LAS) and HL demonstrated the best behavior, but it was

not significant compared with Control asphalt mix

RAP, SBS, and PPA+HL mixes resulted in a significant reduction in moisture resistance

compared with Control asphalt mix

TSR, Table 7.14:

All additives/modifiers and RAP improved moisture resistance significantly compared

with Control asphalt mix, with preference to LAS (SBS+LAS and Control+LAS)

followed by HL (Control+HL)

7.3.4 4 hrs short-term aging and IDOT conditioning

E* Ratio, Table 7.7:

No significant difference between Control asphalt mix and the other asphalt mixes,

except for SBS, RAP, and LAS asphalt mixes

SBS and RAP asphalt mixes reduced moisture resistance significantly while LAS

(Control+LAS) resulted in the best moisture resistance compared with Control asphalt

mix

TSR, Table 7.15:

No significant difference between Control asphalt mix and the other asphalt mixes,

except for PPA+HL mix. All asphalt mixes improved moisture resistance, albeit

insignificantly, compared with Control asphalt mix, especially LAS (SBS+LAS).

PPA+HL was the only mix to significantly reduce moisture resistance compared with

Control asphalt mix. SBS+LAS mix demonstrated the best improvement, but it was not

significant compared to Control asphalt mix

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7.3.5 4 hrs short-term aging and 3 FT conditioning

E* Ratio, Table 7.8:

This case had exactly the same trend as the previous case

TSR, Table 7.16:

LAS (SBS+LAS and Control+LAS) and HL (Control+HL) additives resulted in the best

performance amongst the other asphalt mixes compared to the Control asphalt mix

The other mixes were not significantly different compared with Control asphalt mix

7.3.6 4 hrs short-term aging and 5 FT conditioning

E* Ratio, Table 7.9:

Asphalt mixes show significant moisture resistance improvement compared to Control

asphalt mix, except for Control+HL and SBS mixes

Control+HL and SBS asphalt mixes show no significant difference compared with

Control asphalt mix

PPA + HL and Control+LAS showed the best performance among the asphalt mixes

TSR, Table 7.17:

All mixes showed significant moisture resistance improvement with respect to Control

asphalt mix, except for Control+HL and RAP mixes

Control+HL and RAP asphalt mixes showed no significant difference compared with

Control asphalt mix.

LAS mixes (SBS + LAS and Control + LAS) showed the best performance

The performance-based comparison outcomes from the above six cases are presented in Table

7.18 and Table 7.19 for simplicity. Table 7.18 displays the impact of the additives, modifiers and

RAP in reference to the control mix for the first three cases (1 hr aging). Similar data are

presented in Table 7.19; but for cases 4, 5 and 6 (4 hrs aging). In Table 7.18 and Table 7.19, the

notion N, SR, and SI stand for no impact, significant reduction, and significant improvement,

respectively.

Cases 1, 2, and 3:

In these cases, the significant difference between the outcomes from E* Ratio and TSR is

evident. Generally, TSR values showed significant improvement in moisture resistance when

selected additives, modifiers and RAP were added. However, E* Ratio generally showed no

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improvement; and some cases significant reduction in moisture resistance when same additives,

modifiers, and RAP are included. This indicates that TSR parameter is capable of identifying the

impact of additives/modifiers and RAP on moisture susceptibility than the E* Ratio parameter.

However, although inaccurate, E* Ratio parameter could be more appropriate than using the

master curve to evaluate moisture damage for asphalt mixes.

Cases 4, 5, and 6:

Results from TSR Case 4 showed that it is difficult to capture the impact of additives/modifiers

and RAP on moisture susceptibility after 4 hours of short-term aging under low-conditioning

level (IDOT conditioning). This finding supports the need for excessive conditioning to be able

to distinguish between the moisture susceptibility of different asphalt mixes.

E* Ratio Cases 4 and 5 show the same trend as the previous three cases, but with a different

ranking. The RAP mix still produced the poorest performance with respect to E* Ratio. LAS

(Control+LAS and SBS+LAS) and HL (Control+HL) showed the best performance at TSR Case

5 compared to Control asphalt mix. Control+LAS also in E* Ratio Cases 5 and 6 showed the

best performance with respect to Control mix followed by Control+HL.

In Case 6, both tests showed that four asphalt mixes improved moisture resistance with respect to

Control asphalt mix, while the others had no significant impact. In addition, both tests showed

that Control+HL did not improve moisture resistance significantly with respect to Control

asphalt mix. However, a great deal of variation was observed in the asphalt mix performance

ranking from both tests, such as the case of RAP, SBS, and SBS+LAS asphalt mixes.

Overall, cases 4, 5, and 6 show that E* Ratio and TSR values are in agreement after 4 hrs aging;

especially at 5 FT (excessive) conditioning. Both parameters generally show significant

improvement for Control+LAS, no impact for Control+HL due to the addition of HL, and the

transition of no improvement to significant improvement for SBS+LAS and PPA+HL, especially

with the conditioning increase. The E* Ratio parameter becomes more sensitive to moisture

damage when asphalt concrete specimens are exposed to both excessive aging and conditioning.

Correlation between TSR and E* Ratio was conducted for each mix at the six conditioning cases.

Seven asphalt mixes were considered, which result in a total of 42 cases. The correlation analysis

was conducted using SPSS by running Paired-Samples t Test. When the p-value is equal or more

than 0.05, the difference between the E* Ratio and TSR is insignificant. The correlation results

are presented in Table 7.20.

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At least 80% of the 42 cases show that E* Ratio and TSR is significantly different. This is a clear

indication that E* Ratio is not a proper suitable replacement for TSR to assess asphalt mixture

moisture damage.

This is in agreement with earlier discussion; moisture damage is more pronounced in tension

tests than in compression tests. Material characteristics are different in tension (Lottman test)

than in compression (dynamic modulus).

It is concluded that the E* Ratio parameter is ineffective as moisture damage indicator; hence,

will be excluded in the next section, in which TSR and SFE test results are compared. The

comparison considered the impact of additives, modifiers, and RAP (performance-based) on

moisture susceptibility.

7.4 SFE VS. MIXTURE-LEVEL TESTS

Two limitations should be recognized before comparing SFE and mixture-level tests. The

first limitation relates to aging and the second to conditioning. SFE asphalt binders were tested at

three aging levels: virgin, RTFO, and PAV. In this study, the asphalt mixes were short-term aged

prior to being tested using the modified Lottman and dynamic modulus tests. According to

IDOT, short-term aging of the asphalt mix is simulated after 1 hr at mixing temperature. Per

AASHTO specifications, 4 hrs at 135°C simulate the asphalt mix short-term aging impact. There

was no long-term aging considered at the mixture level. Therefore, TSR was only compared with

the total SFE measured after RTFO aging. The SFE results at virgin and PAV aging were

ignored at this stage.

SFE asphalt binder samples were tested immediately after preparation for total SFE and SFE

components. No conditioning was applied on the SFE samples. TSR was based on sample

conditioning (IDOT, 3 FT, and 5 FT). Despite this limitation, a comparison was conducted

between SFE and TSR since they are all used to evaluate the moisture susceptibility of asphalt

mixes. In the future, a conditioning procedure should be introduced for SFE samples. SFE

samples could be placed in humidity chamber for a specific period of time before measuring the

SFE energy. Then, an SFE ratio of post-conditioning SFE to pre-conditioning SFE could be

established.

Figure 7.1 displays total SFE for asphalt binders at RTFO aging. RAP, Control+LAS,

Control+HL, and SBS+LAS all improved SFE with respect to Control asphalt binder. PPA+HL

showed no improvement with respect to Control asphalt binder. SBS reduced SFE with respect

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to Control asphalt binder. The SFE findings are compared with the six cases in the previous

section.

Case 1 TSR:

Control+LAS: improved significantly with respect to Control asphalt mix. Similar to SFE

result.

Control+HL: insignificant with respect to Control asphalt mix. Not similar to SFE result.

PPA+HL: improved significantly with respect to Control asphalt mix. Not similar to SFE

result.

SBS: improved significantly with respect to Control asphalt mix. Not similar to SFE

result.

SBS+LAS: improved significantly with respect to Control asphalt mix. Similar to SFE

result.

RAP: insignificant with respect to Control asphalt mix. Not similar to SFE result.

Case 2 TSR:

Control+LAS: improved significantly with respect to Control asphalt mix. Similar to SFE

result.

Control+HL: improved significantly with respect to Control asphalt mix. Similar to SFE

result.

PPA+HL: improved significantly with respect to Control asphalt mix. Not similar to SFE

result.

SBS: improved significantly with respect to Control asphalt mix. Not similar to SFE

result.

SBS+LAS: improved significantly with respect to Control asphalt mix. Similar to SFE

result.

RAP: improved significantly with respect to Control asphalt mix. Similar to SFE result.

Case 3 TSR:

Control+LAS: improved significantly with respect to Control asphalt mix. Similar to SFE

result.

Control+HL: improved significantly with respect to Control asphalt mix. Similar to SFE

result.

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PPA+HL: improved significantly with respect to Control asphalt mix. Not similar to SFE

result.

SBS: improved significantly with respect to Control asphalt mix. Not similar to SFE

result.

SBS+LAS: improved significantly with respect to Control asphalt mix. Similar to SFE

result.

RAP: improved significantly with respect to Control asphalt mix. Similar to SFE result.

Case 4 TSR:

Control+LAS: insignificant with respect to Control asphalt mix. Not similar to SFE

result.

Control+HL: insignificant with respect to Control asphalt mix. Not similar to SFE result.

PPA+HL: reduced significantly with respect to Control asphalt mix. Not similar to SFE

result.

SBS: improved significantly with respect to Control asphalt mix. Not similar to SFE

result.

SBS+LAS: improved significantly with respect to Control asphalt mix. Similar to SFE

result.

RAP: insignificant with respect to Control asphalt mix. Not similar to SFE result.

Case 5 TSR:

Control+LAS: insignificant with respect to Control asphalt mix. Not similar to SFE

result.

Control+HL: improved significantly with respect to Control asphalt mix. Similar to SFE

result.

PPA+HL: insignificant with respect to Control asphalt mix. Similar to SFE result.

SBS: insignificant with respect to Control asphalt mix. Not similar to SFE result.

SBS+LAS: improved significantly with respect to Control asphalt mix. Similar to SFE

result.

RAP: insignificant with respect to Control asphalt mix. Not similar to SFE result.

Case 6 TSR:

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Control+LAS: improved significantly with respect to Control asphalt mix. Similar to SFE

result.

Control+HL: insignificant with respect to Control asphalt mix. Not similar to SFE result.

PPA+HL: improved significantly with respect to Control asphalt mix. Not similar to SFE

result.

SBS: improved significantly with respect to Control asphalt mix. Not similar to SFE

result.

SBS+LAS: improved significantly with respect to Control asphalt mix. Similar to SFE

result.

RAP: insignificant with respect to Control asphalt mix. Not similar to SFE result.

In the previous six cases, there are sixteen incidents where TSR is similar to SFE: Case 1

(Control+LAS and SBS+LAS), Case 2 (Control+LAS, Control+HL, SBS+LAS, and RAP), Case

3 (Control+LAS, Control+HL, SBS+LAS, and RAP), Case 4 (SBS+LAS), Case 5 (Control+HL,

PPA+HL, and SBS+LAS), and Case 6 (Control+LAS and SBS+LAS). Fifteen out of the sixteen

incidents are related to the asphalt binders that resulted in significant improvement in moisture

resistance compared with Control asphalt binder (SBS+LAS, Control+LAS, Control+HL, and

RAP). Both tests clearly showed the positive impact of the additive (HL and LAS) when added

to unmodified or modified binders.

The cases with most similarities between SFE and TSR are Cases 2 and 3, where each

demonstrated four similarities. Cases 2 and 3 were conditioned with 3 FT and 5 FT, respectively.

The same explanation can be offered for cases 5 and 6 with comparison to case 4. This supports

the necessity of considering excessive conditioning in tests that evaluate the moisture

susceptibility of asphalt mixes. Excessive conditioning provides more realistic results.

Despite the similarity between SFE and TSR, there is a difference in performance ranking. In

SFE, the best performance was for RAP, then for both Control+LAS and Control+HL, and

finally SBS+LAS. This was not the case for asphalt mixes. The reasons behind this difference in

ranking could be attributed to the influence of conditioning, modified Lottman test failure

mechanism (indirect tensile), and interaction between aggregate and asphalt binder in the

asphalt-mix level. These reasons were not considered in the component level.

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7.5 SUMMARY

The comparison of a component level parameter (SFE) with mixture-level parameter

(TSR) showed that TSR and SFE are efficient in identifying the impact of additives on the

moisture susceptibility of asphalt mixes and asphalt binders. However, E* Ratio appears to have

a potential for qualitatively evaluating moisture damage of asphalt mixes at excessive

conditioning. Results showed that adding LAS and HL are effective in reducing moisture

susceptibility of asphalt mixtures.

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Chapter 7 Figures and Tables

Figure 7.1 SFE results of asphalt binders for RTFO aging level.

33.036.1 36.1

32.931.4

34.3

39.1

0.0

5.0

10.0

15.0

20.0

25.0

30.0

35.0

40.0

Control Control+LAS Control+HL PPA+HL SBS SBS+LAS RAP

SFE

(en

ergy

/cm

2)

RTFO

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Table 7.1 E* Ratio (%) for Control Asphalt Mixture after 1hr Short-term Aging (a) Dynamic

Modulus at All Conditioning Levels (b) E* Ratio Calculation

(a)

Frequency

Dynamic Modulus (E*) at 1 hr Aging- MPa

Unconditioned

(ksi)

IDOT

(ksi)

3 FT

(ksi)

5 FT

(ksi)

25 9771.4 8386.7 7693.0 7317.3

10 8104.5 6856.3 6327.9 6019.1

5 6889.1 5802.6 5373.6 5079.9

1 4458.1 3707.4 3463.3 3230.0

0.5 3613.5 2992.0 2803.5 2607.4

0.1 2038.7 1680.7 1560.9 1481.0

(b)

Frequency E* Ratio (%)

IDOT (%) 3 FT (%) 5 FT (%)

25 8386.7/9771.4=0.86 7693.0/9771.4=0.79 7317.3/9771.4=0.75

10 0.85 0.78 0.74

5 0.84 0.78 0.74

1 0.83 0.78 0.72

0.5 0.83 0.78 0.72

0.1 0.82 0.77 0.73

Average 0.84 0.78 0.73

Table 7.2 E* Ratio for Asphalt Mixtures after 1 hr Short-term Aging

Asphalt Mixture IL

(%)

3 FT

(%)

5 FT

(%)

Control 0.84 0.78 0.73

Control+LAS 0.88 0.72 0.68

Control+HL 0.89 0.91 0.75

PPA+HL 0.81 0.76 0.65

SBS 0.81 0.73 0.64

SBS+LAS 0.91 0.68 0.68

RAP 0.67 0.70 0.65

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Table 7.3 E* Ratio for Asphalt Mixtures after 4 hrs Short-term Aging

Asphalt Mixture IL

(%)

3 FT

(%)

5 FT

(%)

Control 0.87 0.82 0.58

Control+LAS 1.21 1.14 0.72

Control+HL 0.94 0.90 0.58

PPA+HL 0.89 0.86 0.85

SBS 0.73 0.62 0.61

SBS+LAS 0.84 0.74 0.67

RAP 0.76 0.63 0.67

Table 7.4 E* Ratio (%) Statistical Analysis for Asphalt Mixes at IDOT Conditioning after 1 hr

Aging

Table 7.5 E* Ratio (%) Statistical Analysis for Asphalt Mixes at 3 FT Conditioning after 1 hr

Aging

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Table 7.6 E* Ratio (%) Statistical Analysis for Asphalt Mixes at 5 FT Conditioning after 1 hr

Aging

Table 7.7 E* Ratio (%) Statistical Analysis for Asphalt Mixes at IDOT Conditioning after 4 hrs

Aging

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Table 7.8 E* Ratio (%) for Statistical Analysis Asphalt Mixes at 3 FT Conditioning after 4 hrs

Aging

Table 7.9 E* Ratio (%) Statistical Analysis for Asphalt Mixes at 5 FT Conditioning after 4 hrs

Aging

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Table 7.10 TSR (%) Results for Asphalt Mixes after 1 hr Aging

Mix TSR 1h-IDOT

(%)

TSR 1h-3 FT

(%)

TSR 1h-5 FT

(%)

Control 82.0 59.8 45.2

LAS Mix 97.2 89.3 85.7

HL Mix 80.1 77.7 74.8

PPA+HL Mix 90.5 73.1 60.7

SBS Mix 98.1 80.0 59.9

SBS+LAS Mix 99.7 92.4 88.6

RAP Mix 87.4 77.0 66.9

Table 7.11 TSR (%) Results for Asphalt Mixes after 4 hrs Aging

Mix TSR 4h-IDOT

(%)

TSR 4h-3 FT

(%)

TSR 4h-5 FT

(%)

Control 88.0 63.1 45.2

LAS Mix 91.3 74.7 63.5

HL Mix 91.0 83.7 57.8

PPA+HL Mix 68.6 65.4 62.6

SBS Mix 94.9 72.0 59.2

SBS+LAS Mix 97.7 88.0 84.0

RAP Mix 84.5 63.3 53.8

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Table 7.12 TSR (%) Statistical Analysis for Asphalt Mixes at IDOT Conditioning after 1 hr

Aging

Table 7.13 TSR (%) Statistical Analysis for Asphalt Mixes at 3 FT Conditioning after 1 hr Aging

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Table 7.14 TSR (%) Statistical Analysis for Asphalt Mixes at 5 FT Conditioning after 1 hr Aging

Table 7.15 TSR (%) Statistical Analysis for Asphalt Mixes at IDOT Conditioning after 4 hrs

Aging

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Table 7.16 TSR (%) Statistical Analysis for Asphalt Mixes at 3 FT Conditioning after 4 hrs

Aging

Table 7.17 TSR (%) Statistical Analysis for Asphalt Mixes at 5 FT Conditioning after 4 hrs

Aging

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Table 7.18 Impact of additives, modifiers, and RAP with respect to Control Mix after 1 hr aging

and adopted conditioning levels (IDOT, 3FT, and 5FT)

Case RATIO CONT. +

LAS

CONT. +

HL PPA+HL SBS

SBS +

LAS RAP

1hr+IDOT ESR N SI N N SI SR

TSR SI N SI SI SI N

1hr+3FT ESR N SI N N SR SR

TSR SI SI SI SI SI SI

1hr+5FT ESR N N SR SR N SR

TSR SI SI SI SI SI SI

Table 7.19 Impact of additives, modifiers, and RAP with respect to Control Mix after 4 hrs aging

and adopted conditioning levels (IDOT, 3FT, and 5FT)

Case RATIO CONT. +

LAS

CONT. +

HL PPA+HL SBS

SBS +

LAS RAP

4hr+IDOT ESR SI N N SR N SR

TSR N N SR N N N

4hr+3FT ESR SI N N SR N SR

TSR SI SI N N SI N

4hr+5FT ESR SI N SI N SI SI

TSR SI N SI SI SI N

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Table 7.20 E* Ratio and TSR correlation for asphalt mixes at considered aging and conditioning levels

Asphalt Mix Parameter

1 hr and IDOT 1 hr and 3FT 1 hr and 5FT 4 hr and IDOT 4 hr and 3FT 4 hr and 5FT

E*

Ratio

(%)

TSR

(%)

E*

Ratio

(%)

TSR

(%)

E*

Ratio

(%)

TSR

(%)

E*

Ratio

(%)

TSR

(%)

E*

Ratio

(%)

TSR

(%)

E*

Ratio

(%)

TSR

(%)

Control

Average 83.83 81.9 77.78 55.9 73.37 41.9 87.47 87.9 82.35 63.1 58.30 45.5

Stand. Dev. 1.27 5.3 0.70 6.32 1.10 5.14 6.29 1.45 6.16 4.43 2.79 2.05

p-value 0.41 0.0 0.0 0.85 0.002 0.0

Difference Insignificant Significant Significant Insignificant Significant Significant

Control+LAS

Average 87.63 97.2 72.15 89.3 67.55 85.7 121.0 91.3 114.3 74.7 72.37 63.5

Stand. Dev. 7.36 0.45 8.71 6.09 8.58 8.85 8.78 4.28 10.24 7.33 1.33 1.55

p-value 0.022 0.01 0.006 0.001 0.001 0.0

Difference Significant Significant Significant Significant Significant Significant

Control+HL

Average 83.83 81.97 77.78 55.97 73.37 41.97 87.47 87.97 82.35 63.10 58.3 45.50

Stand. Dev. 1.27 5.30 0.70 6.32 1.10 5.14 6.29 1.45 6.16 4.43 2.79 2.05

p-value 0.41 0.0 0.0 0.85 0.002 0.0

Difference Insignificant Significant Significant Insignificant Significant Significant

Control+PPA

+HL

Average 80.5 90.53 76.48 73.07 65.37 60.73 89.47 68.63 86.42 65.37 84.82 62.60

Stand. Dev. 2.89 0.39 0.88 3.75 3.21 0.65 0.57 1.65 1.87 1.08 0.92 6.59

p-value 0.0 0.10 0.022 0.0 0.0 0.001

Difference Significant Insignificant Significant Significant Significant Significant

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Table 7.20 (cont.)

Control+SBS

Average 81.0 98.07 73.0 80.0 63.55 60.00 72.6 94.8 62.3 72.03 60.7 59.17

Stand. Dev. 0.52 2.04 1.71 5.66 0.87 1.00 3.54 2.73 2.44 1.04 1.91 3.04

p-value 0.0 0.019 0.0 0.0 0.0 0.382

Difference Significant Significant Significant Significant Significant Insignificant

Control+SBS

+LAS

Average 91.4 99.70 68.52 92.40 68.23 88.57 83.70 97.73 73.73 88.00 66.67 84.00

Stand. Dev. 1.15 .70 1.83 1.83 1.71 4.79 0.87 5.04 1.12 3.94 2.55 6.56

p-value 0.0 0.0 0.0 0.001 0.0 0.001

Difference Significant Significant Significant Significant Significant Significant

Control+RAP

Average 67.17 87.40 70.17 77.00 65.33 66.87 75.63 84.47 62.50 63.23 67.07 53.77

Stand. Dev. 5.85 1.00 4.67 3.35 4.13 2.85 5.45 4.10 6.18 4.08 5.65 1.50

p-value 0.0 0.018 0.378 0.037 0.845 0.004

Difference Significant Significant Insignificant Significant Insignificant Significant

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CHAPTER 8 SUMMARY, CONCLUSION AND RECOMMENDATIONS

The main objective of this study is to predict the impact of several additives/modifiers

and recycled asphalt pavement (RAP) on moisture susceptibility of asphalt concrete through

mixture-level and component-level testing. The impact was evaluated under different aging and

conditioning levels. A checkup for correlation was organized within mixture-level tests and

between mixture- and component-level tests.

Mixes with one aggregate, control binder, two additives, two modifiers, and RAP were used. The

aggregate is dolomitic limestone; the control binder has a performance grade (PG) of 64-22; the

additives are liquid anti-stripping (LAS) agent and hydrated lime (HL); and the modifiers are

polyphosphoric acid (PPA) and styrene butadiene styrene (SBS). Seven mixes were prepared

from the control binder and selected additives, modifiers, and RAP: Control mix, Control mix

with LAS, Control mix with HL, Control mix with SBS, Control mix with SBS and LAS,

Control mix with PPA and HL, and Control mix with RAP.

Two mixture-level tests were used to evaluate the moisture resistance of asphalt mixes: modified

Lottman test (AASHTO T283) and complex modulus test (AASHTO T 342). Two aging

durations and four conditioning periods were considered for the mixture-level tests. The two

aging durations are 1 hr at 155°C (311°F) and 4 hrs at 135°C (275°F). The conditioning periods

are unconditioned (dry), IDOT conditioning, 3 freezing and thawing (FT) cycles, and 5 FT

cycles.

Seven asphalt binders and two aggregate types were used for the component-level tests. The

seven asphalt binders were: Control asphalt binder, Control+LAS asphalt binder, Control+HL

asphalt binder, Control+SBS (SBS) asphalt binder, Control+SBS+LAS (SBS+LAS) asphalt

binder, Control+PPA+HL (PPA+HL) asphalt binder, Control+RAP (RAP) asphalt binder. The

aggregate types were dolomitic limestone and lime. The SFE and adhesion (DAT and BT) tests

represent the component-level types. Aging was considered at the component-level by using the

rolling thin film oven (RTFO) and pressure aging vessel (PAV).

8.1 FINDINGS

The key findings of this study are summarized as follows:

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8.1.1 Modified Lottman Test (AASHTO T 283)

Despite the conditioning period, IDT strength after 4 hrs of aging was higher than that

after 1 hr of aging, and TSR was lower after 4 hrs of aging compared with 1 hr of aging.

IDT strength and TSR decreased with more conditioning within the same aging period.

The RAP, additives, and modifiers considered in this study improved the IDT strength

compared with the Control mix with preference to RAP, except for LAS which

demonstrated some softening in the unconditioned state after 1 hr aging.

The IDT strength of Control+LAS asphalt mix showed no softening impact at the

unconditioned state after 4 hrs aging as a result of adding LAS, compared with the

Control asphalt mix. Additional aging increased mixture stability when LAS was added.

In the conditioned state (IDOT, 3 FT cycles, and 5 FT cycles), the Control+LAS asphalt

mix always had higher IDT strength compared with Control asphalt mix. This indicates

the ability of the LAS additive to better sustain the mix strength after conditioning. The

IDT strength reduction rate with the increase in conditioning for the Control+LAS, 1 hr

aged mix was lower compared with the rate after 4 hrs aging.

The influence of LAS additive when added to the SBS-modified mix after 1 hr and 4 hrs

aging in the unconditioned state showed no significant alteration compared with the SBS

mix. In the conditioned state, (IDOT, 3 FT cycles, and 5 FT cycles), the SBS+LAS

asphalt mix always had higher IDT strength compared with SBS asphalt mix.

PPA+HL asphalt mix after 1 hr aging had higher IDT with respect to HL asphalt mix in

all cases except after 5 FT cycles conditioning. PPA+HL asphalt mix after 4 hrs aging

had lower IDT with respect to HL asphalt mix in all cases, except after 5 FT cycles

conditioning. Despite aging duration, there was no significant difference in the IDT

strength between PPA+HL and HL mixes after 5 FT cycles.

There is a significant difference between the IDT measured after 1 hr and 4 hrs aging for

all mixes in the unconditioned (dry) and IDOT (IL) conditioning stage, except for mixes

with RAP. After 3 FT cycles, the soft mixes (Control, LAS, and HL) showed a significant

difference between IDT 1 hr and IDT 4 hrs, except for the stiffer mixes (PPA+HL, SBS,

SBS+LAS, and RAP). As for the 5 FT cycles, both soft and stiff mixes showed an

insignificant difference between IDT 1 hr and IDT 4 hrs.

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The aging duration (1 hr vs. 4 hrs) had no influence on the moisture susceptibility of

almost all asphalt mixes after IDOT and 3 FT conditioning. Control, PPA+HL, SBS, and

SBS+LAS asphalt mixes showed no significant differences between TSR at 1 hr and 4

hrs after 5 FT conditioning. However, there was a significant difference in moisture

susceptibility for mixes with LAS, HL, and RAP after 5 FT conditioning.

8.1.2 Complex Modulus (AASHTO T 342)

More conditioning resulted in a drop in stiffness despite aging duration (1 hr and 4 hrs).

Stiffness after 4 hrs aging was higher than the stiffness measured after 1 hr aging.

The difference in stiffness between conditioning levels was obvious at low frequency

(high temperature) while no significant difference was observed at the high frequency

(low temperature).

The difference between the master curves as a result of conditioning at the same aging

duration was insignificant. The difference in stiffness after 4 hrs aging and 1 hr aging was

insignificant in the modified mixes (PPA+HL, SBS and SBS+LAS) and RAP mix. This

was not the case for the unmodified mixes (Control, Control+LAS, and Control+HL).

The RAP mix seemed to produce the highest stiffness amongst the asphalt mixes at all

aging and conditioning levels.

It is very difficult to rank and evaluate the effect of modifiers and additives at the

different aging and conditioning levels for the other mixes using master curves.

8.1.3 Surface Free Energy

The total SFE and SFE components of asphalt binders agree with the typical magnitude

of SFE components.

The nonpolar Lifschitz-van der Waals (LW) and basic components had the major

contribution to both works of adhesion and cohesion.

Aggregate had higher SFE compared with asphalt binder. Aggregate had a significantly

higher base component compared with its acid component.

LAS and HL improved moisture resistance because both had increased work of adhesion

and cohesion. However, the impact of LAS decreased with aging while that of HL

increased. The impact of LAS and HL was observed in spite of the fact that they were

added to unmodified asphalt binder (Control) and modified asphalt binder (SBS-modified

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and PPA-modified). However, the modified asphalt binder with LAS, such as SBS+LAS,

seemed to have better resistance to aging (SBS+LAS SFE at RTFO showed similar

results to SBS+LAS SFE at PAV).

Control+LAS at PAV almost had the same SFE and work of adhesion and cohesion for

the Control asphalt binder.

RAP improved moisture resistance because both had increased work of adhesion and

cohesion. The influence of RAP decreased with aging. The scenarios prepared with RAP

at RTFO and PAV had no significant difference in performance.

The SFE of control and SBS-modified asphalt binders and work of adhesion and

cohesion barely changed with aging. This was not the case for control asphalt binder at

PAV where the high-base component resulted in higher work of adhesion compared with

RTFO and virgin levels.

Work of adhesion and cohesion follow the same trend as SFE. The higher the SFE, the

higher the work of adhesion and cohesion and vice versa.

8.1.4 Direct Adhesion Test

LAS-modified asphalt binders improved the adhesion performance significantly while

RAP significantly reduced the adhesion performance compared with Control asphalt

binder.

LAS-modified asphalt binder had the highest E while RAP produced the lowest E.

HL and SBS neither improved nor reduced significantly the adhesion performance

compared with Control asphalt binder.

Except for Control asphalt binder, there was no significant differences when comparing

the performance at virgin with RTFO for each asphalt binder.

8.1.5 Blister Test

All asphalt binders failed the BT test because no separation occurred between any of the

tested asphalt binders and the aluminum substrate.

8.1.6 Mixture-Level Tests Correlation

Almost half of the asphalt mixes did not result in any significance changes in moisture

resistance for the Control asphalt mix when considering E* Ratio.

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The difference between TSR and E* Ratio was mainly in the ranking of asphalt mixes

based on their performance, especially in the case of the RAP asphalt mix which

significantly reduced the moisture resistance of the Control asphalt mix considering E*

Ratio. On the other hand, RAP significantly improved moisture resistance of the Control

asphalt mix.

Despite the difference in ranking, both parameters (TSR and E* Ratio) showed the

significant improvement achieved by LAS especially when added to Control asphalt mix.

It was also observed that HL (Control+HL) had no significant impact after excessive

aging and conditioning (4 hrs and 5 FT).

There are differences in asphalt mixes performance between 1 hr and 4 hrs short-term

aging considering E* Ratio threshold. On the other hand, TSR showed similarities in the

performance of asphalt mixes between 1 hr and 4 hrs short-term aging.

8.1.7 Mixture and Component-Level Tests Correlation

E* Ratio parameter is ineffective as moisture damage indicator.

Moisture damage is more pronounced in tension tests than in compression tests

TSR had good correlation with SFE results.

The best correlation between TSR and SFE occurred at 3 and 5 FT conditioning levels.

8.2 CONCLUSIONS

The conclusions obtained from this study are summarized below:

Indirect tensile ration (TSR) and surface free energy (SFE) can successfully be used to

determine moisture damage. However, dynamic modulus of AC mixture, binder blister

test, and binder direct tensile test are not effective in evaluating potential moisture

damage in AC mixtures because they are not sensitive to moisture conditioning.

Reclaimed asphalt pavements (RAP), additives, and modifiers considered in this study

generally improved tensile strength and moisture resistance of AC mixtures. As the aging

of AC increases, its tensile strength and stiffness become greater despite conditioning.

The difference in AC mixtures strength due to aging becomes insignificant with the

increase in conditioning. However, applying more freezing and thawing (FT) cycles

(conditioning) results in lowering AC tensile strength and stiffness despite the aging

period.

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Moisture susceptibility can be best evaluated using the modified Lottman test, especially

when extensive conditioning is considered, at 4 hrs aging with 5 FT conditioning.

Based on the surface free energy, hydrated lime (HL) is efficient in reducing moisture

susceptibility even after aging. It worked well when PPA is added to reduce aging effect.

While liquid antistripping (LAS) agent improved the moisture resistance of both

unmodified and polymer-modified AC mixes, its effect diminishes with aging. On the

other hand, while SBS and RAP increase AC stiffness, they had minimum effect on

reducing AC moisture susceptibility compared with LAS and HL.

Both TSR and SFE are efficient in identifying the impact of additives on the moisture

susceptibility of AC mixes and asphalt binders. On the other hand, dynamic modulus

ratio (E* Ration) appears to detect AC potential moisture damage susceptibility only at

excessive conditioning.

8.3 IMPACT OF THE STUDY

The impact of this study can be summarized as follows:

1. This study provides directions to the best practice of predicting AC potential damage and

optimum modifiers to control the damage.

2. The dynamic modulus test through its parameter, master curve and E* Ratio, is not

appropriate to evaluate moisture susceptibility of AC mixtures.

3. Surface free energy could be an effective approach to predict adhesion and cohesion

characteristics of AC mix components. In addition, Sessile drop device could capture the

aging impact on surface free energy parameters.

4. Using SBS and LAS in AC mix could improve both its stiffness and moisture resistance.

5. The shelf time of LAS should be identified as it may become ineffective after a specific

storage period as shown in surface free energy test results.

8.4 RECOMMENDATIONS

The recommendations derived from this study are summarized below:

Proper conditioning is recommended to be able to distinguish between the moisture

susceptibility of different asphalt mixes. The best correlation between SFE and TSR was

observed after extensive conditioning (3 FT and above). Results from modified Lottman

based on limited conditioning level (IDOT conditioning) may not capture the impact of

moisture accurately.

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Adequate aging time and process need to be identified for proper condition of tested

specimens.

In this study, only course asphalt mixes (19mm NMAS) were considered. It is

recommended that other types of asphalt mixes be considered such as open graded, fine

mixes, warm mixes, and stone mastic asphalt mixes in order to better evaluate and

validate the findings of this study.

A study on asphalt binder chemistry and its relationship to moisture damage is

recommend to better understand SFE results and the impact of aging.

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APPENDIX A: SURFACE FREE ENERGY DETAILED MEASUREMENTS

Table A.1 Probe liquids total SFE and SFE components

Liquid Total SFE LW Acid Base

Water 72.8 21.8 25.5 25.5

Glycerol 63.6 34.2 16.6 13.1

Diiodo 50.8 50.8 0.0 0.0

Table A.2 Control asphalt binder contact angles with probe liquids

Control Asphalt Binder

Liquid Virgin RTFO PAV

Water 97.0 98.7 92.3

Glycerol 87.9 88.7 90.5

Diiodo 54.8 53.8 57.4

Note: All contact angles has a standard deviation ≤1

Table A.3 Control+LAS asphalt binder contact angles with probe liquids

Control+LAS Asphalt Binder

Liquid Virgin RTFO PAV

Water 85.2 91.9 94.6

Glycerol 92.2 91.8 90.2

Diiodo 58.0 55.6 56.2

Note: All contact angles has a standard deviation ≤1

Table A.4 Control+HL asphalt binder contact angles with probe liquids

Control+HL Asphalt Binder

Liquid Virgin RTFO PAV

Water 96.8 96.6 97.0

Glycerol 92.1 91.5 91.8

Diiodo 57.2 52.0 52.1

Note: All contact angles has a standard deviation ≤1

Table A.5 PPA+HL asphalt binder contact angles with probe liquids

PPA+HL Asphalt Binder

Liquid Virgin RTFO PAV

Water 96.8 97.6 94.2

Glycerol 91.6 90.0 92.3

Diiodo 57.6 55.2 51.9

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Table A.6 SBS asphalt binder contact angles with probe liquids

SBS Asphalt Binder

Liquid Virgin RTFO PAV

Water 95.9 98.4 98.1

Glycerol 89.6 91.5 91.4

Diiodo 56.9 58.0 58.1

Note: All contact angles has a standard deviation ≤1

Table A.7 SBS+LAS asphalt binder contact angles with probe liquids

SBS+LAS Asphalt Binder

Liquid Virgin RTFO PAV

Water 88.5 97.7 96.2

Glycerol 93.4 92.2 92.1

Diiodo 57.7 54.6 55.1

Note: All contact angles has a standard deviation ≤1

Table A.8 RAP asphalt binder contact angles with probe liquids

RAP Asphalt Binder

Liquid

Virgin

Control

+

Virgin

RAP

RTFO

Control +

Virgin

RAP

RTFO

Control +

RTFO

RAP

PAV

Control +

PAV RAP

(No RTFO)

PAV Control

+ PAV RAP

(with RTFO)

Water 87.9 90.1 88.9 94.2 93.5

Glycerol 88.0 87.5 87.6 90.4 89.9

Diiodo 51.4 48.7 51.1 53.3 54.4

Note: All contact angles has a standard deviation ≤1

Table A.9 Aggregate contact angles with probe liquids

Liquid Dolomitic Limestone Lime

Water 49.5 52.0

Glycerol 67.5 76.7

Diiodo 22.6 13.4

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APPENDIX B: E* RATIO DETAILED CALCULATIONS

Table B.1 E* Ratio for Control asphalt mixture after 1hr short-term aging (a) Dynamic modulus

at all conditioning levels (b) E* Ratio calculation

(a)

Frequency Dynamic Modulus (E*) - MPa

Uncond. IDOT 3 FT 5 FT

25 9771.4 8386.7 7693.0 7317.3

10 8104.5 6856.3 6327.9 6019.1

5 6889.1 5802.6 5373.6 5079.9

1 4458.1 3707.4 3463.3 3230.0

0.5 3613.5 2992.0 2803.5 2607.4

0.1 2038.7 1680.7 1560.9 1481.0

(b)

Frequency E* Ratio

IDOT 3 FT 5 FT

25 8386.7/9771.4=0.86 7693.0/9771.4=0.79 7317.3/9771.4=0.75

10 0.85 0.78 0.74

5 0.84 0.78 0.74

1 0.83 0.78 0.72

0.5 0.83 0.78 0.72

0.1 0.82 0.77 0.73

Average 0.84 0.78 0.73

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Table B.2 E* Ratio for Control+LAS asphalt mixture after 1hr short-term aging (a) Dynamic

modulus at all conditioning levels (b) E* Ratio calculation

(a)

Frequency Dynamic Modulus (E*) - MPa

Uncond. IDOT 3 FT 5 FT

25 9185.2 8786.8 7664.0 7211.7

10 7345.4 7227.2 6098.6 5759.2

5 7331.6 6134.0 5044.9 4756.4

1 4667.9 3853.3 3103.5 2891.6

0.5 3725.5 3082.7 2381.6 2266.4

0.1 2081.6 1724.6 1400.7 1264.8

(b)

Frequency E* Ratio

IDOT 3 FT 5 FT

25 0.96 0.83 0.79

10 0.98 0.83 0.78

5 0.84 0.69 0.65

1 0.83 0.66 0.62

0.5 0.83 0.64 0.61

0.1 0.83 0.67 0.61

Average 0.88 0.72 0.68

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Table B.3 E* Ratio for Control+HL asphalt mixture after 1hr short-term aging (a) Dynamic

modulus at all conditioning levels (b) E* Ratio calculation

(a)

Frequency Dynamic Modulus (E*) - MPa

Uncond. IDOT 3 FT 5 FT

25 10478.1 9608.7 9682.2 8221.2

10 8686.2 7896.8 7940.1 6720.5

5 7359.8 6698.0 6724.9 5649.5

1 4754.5 4275.4 4324.3 3549.1

0.5 3861.1 3429.0 3490.1 2852.1

0.1 2330.0 1947.8 2076.6 1610.9

(b)

Frequency E* Ratio

IDOT 3 FT 5 FT

25 0.92 0.92 0.78

10 0.91 0.91 0.77

5 0.91 0.91 0.77

1 0.90 0.91 0.75

0.5 0.89 0.90 0.74

0.1 0.84 0.89 0.69

Average 0.89 0.91 0.75

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Table B.4 E* Ratio for PPA+HL asphalt mixture after 1hr short-term aging (a) Dynamic

modulus at all conditioning levels (b) E* Ratio calculation

(a)

Frequency Dynamic Modulus (E*) - MPa

Uncond. IDOT 3 FT 5 FT

25 11680.1 9788.8 9070.2 8107.1

10 9663.4 8030.5 7459.8 6571.4

5 8254.6 6778.8 6330.6 5511.7

1 5424.3 4306.4 4130.8 3478.7

0.5 4435.0 3466.7 3347.7 2784.5

0.1 2528.7 1938.2 1911.5 1544.2

(b)

Frequency E* Ratio

IDOT 3 FT 5 FT

25 0.84 0.78 0.69

10 0.83 0.77 0.68

5 0.82 0.77 0.67

1 0.79 0.76 0.64

0.5 0.78 0.75 0.63

0.1 0.77 0.76 0.61

Average 0.81 0.76 0.65

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Table B.5 E* Ratio for SBS asphalt mixture after 1hr short-term aging (a) Dynamic modulus at

all conditioning levels (b) E* Ratio calculation

(a)

Frequency Dynamic Modulus (E*) - MPa

Uncond. IDOT 3 FT 5 FT

25 10347.4 8445.8 7395.3 6567.2

10 8414.6 6857.8 6035.0 5320.8

5 7086.9 5760.2 5108.0 4469.5

1 4512.1 3635.7 3296.4 2848.2

0.5 3645.7 2925.9 2679.1 2301.7

0.1 2063.1 1673.3 1569.4 1346.8

(b)

Frequency E* Ratio

IDOT 3 FT 5 FT

25 0.82 0.71 0.63

10 0.81 0.72 0.63

5 0.81 0.72 0.63

1 0.81 0.73 0.63

0.5 0.80 0.73 0.63

0.1 0.81 0.76 0.65

Average 0.81 0.73 0.64

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Table B.6 E* Ratio for SBS+LAS asphalt mixture after 1hr short-term aging (a) Dynamic

modulus at all conditioning levels (b) E* Ratio calculation

(a)

Frequency Dynamic Modulus (E*) - MPa

Uncond. IDOT 3 FT 5 FT

25 9687.6 9020.5 6903.9 6858.9

10 7858.5 7253.8 5489.2 5457.8

5 6573.6 6022.7 4520.2 4508.8

1 4109.5 3735.5 2777.5 2764.4

0.5 3309.5 2975.1 2210.0 2211.8

0.1 1853.5 1683.9 1236.1 1231.3

(b)

Frequency E* Ratio

IDOT 3 FT 5 FT

25 0.93 0.71 0.71

10 0.92 0.70 0.69

5 0.92 0.69 0.69

1 0.91 0.68 0.67

0.5 0.90 0.67 0.67

0.1 0.91 0.67 0.66

Average 0.91 0.68 0.68

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Table B.7 E* Ratio for RAP asphalt mixture after 1hr short-term aging (a) Dynamic modulus at

all conditioning levels (b) E* Ratio calculation

(a)

Frequency Dynamic Modulus (E*) - MPa

Uncond. IDOT 3 FT 5 FT

25 15040.3 10883.8 11316.4 10548.9

10 13176.0 9430.2 9723.7 9035.3

5 11808.4 8337.6 8569.0 7964.5

1 8957.6 5932.9 6168.5 5730.1

0.5 7854.9 5069.4 5290.3 4909.9

0.1 5534.5 3150.3 3475.2 3246.2

(b)

Frequency E* Ratio

IDOT 3 FT 5 FT

25 0.72 0.75 0.70

10 0.72 0.74 0.69

5 0.71 0.73 0.67

1 0.66 0.69 0.64

0.5 0.65 0.67 0.63

0.1 0.57 0.63 0.59

Average 0.67 0.70 0.65

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Table B.8 E* Ratio for Control asphalt mixture after 4hrs short-term aging (a) Dynamic modulus

at all conditioning levels (b) E* Ratio calculation

(a)

Frequency Dynamic Modulus (E*) - MPa

Uncond. IDOT 3 FT 5 FT

25 14,084.91 11,229.69 10,540.88 8,708.08

10 11,568.53 9,546.64 8,966.93 7,031.41

5 9,920.71 8,352.08 7,859.03 5,905.47

1 6,542.90 5,883.50 5,530.21 3,722.44

0.5 5,362.55 4,976.08 4,691.72 2,986.45

0.1 3,273.31 3,132.83 2,964.07 1,803.04

(b)

Frequency E* Ratio

IDOT 3 FT 5 FT

25 0.80 0.75 0.62

10 0.83 0.78 0.61

5 0.84 0.79 0.60

1 0.90 0.85 0.57

0.5 0.93 0.87 0.56

0.1 0.96 0.91 0.55

Average 0.87 0.82 0.58

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Table B.9 E* Ratio for Control+LAS asphalt mixture after 4hrs short-term aging (a) Dynamic

modulus at all conditioning levels (b) E* Ratio calculation

(a)

Frequency Dynamic Modulus (E*) - MPa

Uncond. IDOT 3 FT 5 FT

25 10404.45 11450.00 10568.46 7724.82

10 8509.28 9706.39 9044.86 6255.45

5 7239.45 8437.27 7913.01 5271.01

1 4679.59 5840.33 5524.93 3349.12

0.5 3786.56 4904.48 4673.39 2687.16

0.1 2262.52 2974.52 2886.82 1609.71

(b)

Frequency E* Ratio

IDOT 3 FT 5 FT

25 1.10 1.02 0.74

10 1.14 1.06 0.74

5 1.17 1.09 0.73

1 1.25 1.18 0.72

0.5 1.30 1.23 0.71

0.1 1.31 1.28 0.71

Average 1.21 1.14 0.72

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Table B.10 E* Ratio for Control+HL asphalt mixture after 4hrs short-term aging (a) Dynamic

modulus at all conditioning levels (b) E* Ratio calculation

(a)

Frequency Dynamic Modulus (E*) - MPa

Uncond. IDOT 3 FT 5 FT

25 14,521.14 12,595.00 11,820.85 8,305.18

10 12,109.80 10,781.47 10,159.25 6,969.41

5 10,425.20 9,458.74 8,966.46 6,052.67

1 6,924.18 6,682.05 6,435.10 4,091.61

0.5 5,677.49 5,637.06 5,511.50 3,378.48

0.1 3,473.51 3,512.65 3,530.46 2,051.82

(b)

Frequency E* Ratio

IDOT 3 FT 5 FT

25 0.87 0.81 0.57

10 0.89 0.84 0.58

5 0.91 0.86 0.58

1 0.97 0.93 0.59

0.5 0.99 0.97 0.60

0.1 1.01 1.02 0.59

Average 0.94 0.90 0.58

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Table B.11 E* Ratio for PPA+HL asphalt mixture after 4hrs short-term aging (a) Dynamic

modulus at all conditioning levels (b) E* Ratio calculation

(a)

Frequency Dynamic Modulus (E*) - MPa

Uncond. IDOT 3 FT 5 FT

25 11199.21 9986.15 9498.42 9427.85

10 9370.50 8337.28 7961.60 7870.79

5 8048.36 7159.25 6856.50 6770.12

1 5342.87 4778.12 4633.76 4542.45

0.5 4402.47 3951.11 3833.53 3752.20

0.1 2579.55 2334.06 2313.99 2227.59

(b)

Frequency E* Ratio

IDOT 3 FT 5 FT

25 0.89 0.85 0.84

10 0.89 0.85 0.84

5 0.89 0.85 0.84

1 0.89 0.87 0.85

0.5 0.90 0.87 0.85

0.1 0.90 0.90 0.86

Average 0.89 0.86 0.85

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Table B.12 E* Ratio for SBS asphalt mixture after 4hrs short-term aging (a) Dynamic modulus at

all conditioning levels (b) E* Ratio calculation

(a)

Frequency Dynamic Modulus (E*) - MPa

Uncond. IDOT 3 FT 5 FT

25 11526.40 8931.06 7574.86 7342.00

10 9755.93 7358.99 6272.27 6059.28

5 8459.80 6256.88 5324.32 5161.77

1 5769.39 4092.74 3538.70 3430.68

0.5 4826.81 3359.56 2906.76 2832.96

0.1 2884.73 1977.09 1713.35 1713.76

(b)

Frequency E* Ratio

IDOT 3 FT 5 FT

25 0.77 0.66 0.64

10 0.75 0.64 0.62

5 0.74 0.63 0.61

1 0.71 0.61 0.59

0.5 0.70 0.60 0.59

0.1 0.69 0.59 0.59

Average 0.73 0.62 0.61

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Table B.13 E* Ratio for SBS+LAS asphalt mixture after 4hrs short-term aging (a) Dynamic

modulus at all conditioning levels (b) E* Ratio calculation

(a)

(b)

Frequency E* Ratio

IDOT 3 FT 5 FT

25 0.85 0.75 0.70

10 0.84 0.74 0.69

5 0.83 0.74 0.67

1 0.83 0.73 0.65

0.5 0.83 0.73 0.64

0.1 0.84 0.73 0.64

Average 0.84 0.74 0.67

Frequency Dynamic Modulus (E*) - MPa

Uncond. IDOT 3 FT 5 FT

25 10485.62 8915.75 7914.22 7371.60

10 8687.79 7323.92 6465.66 5959.50

5 7390.65 6170.84 5471.08 4985.36

1 4817.75 3997.44 3525.27 3149.74

0.5 3966.18 3275.94 2876.99 2545.45

0.1 2275.88 1906.70 1657.30 1455.84

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Table B.14 E* Ratio for RAP asphalt mixture after 4hrs short-term aging (a) Dynamic modulus

at all conditioning levels (b) E* Ratio calculation

(a)

Frequency Dynamic Modulus (E*) - MPa

Uncond. IDOT 3 FT 5 FT

25 14495.41 11825.36 10120.09 10689.32

10 12818.82 10229.06 8623.99 9158.15

5 11567.23 9055.21 7568.69 8062.73

1 8823.91 6573.02 5355.38 5782.09

0.5 7760.08 5655.88 4557.49 4949.78

0.1 5512.68 3675.98 2924.98 3216.44

(b)

Frequency E* Ratio

IDOT 3 FT 5 FT

25 0.82 0.70 0.74

10 0.80 0.67 0.71

5 0.78 0.65 0.70

1 0.74 0.61 0.66

0.5 0.73 0.59 0.64

0.1 0.67 0.53 0.58

Average 0.76 0.63 0.67