EFFECT OF OVERHEATING ON ADHESION OF

ASPHALT BINDER

Session 2017-2021

Authors
Danish Abdullah 17-CE-60
Usama Mudassar 17-CE-84

Supervisor
Prof. Dr. Naveed Ahmad
(Professor)

DEPARTMENT OF CIVIL ENGINEERING

FACULTY OF CIVIL AND ENVIRONMENTAL ENGINEERING
UNIVERSITY OF ENGINEERING AND TECHNOLOGY, TAXILA

i
 Effect of Overheating on Adhesion of Asphalt Binder

Authors
Danish Abdullah 17-CE-60
Usama Mudassar 17-CE-84

A thesis submitted in partial fulfillment of the requirement for the degree of

B.Sc. Civil Engineering

Thesis Supervisor
Prof. Dr. Naveed Ahmad
(Professor)
Department of Civil Engineering

External Examiner’s Signature __________________________________

Thesis Supervisor’s Signature _____________________________

DEPARTMENT OF CIVIL ENGINEERING

FACULTY OF CIVIL AND ENVIRONMENTAL ENGINEERING
UNIVERSITY OF ENGINEERING AND TECHNOLOGY, TAXILA
JULY 2021

ii
 ABSTRACT

Effect of Overheating on Adhesion of Asphalt Binder

Adhesion of bitumen is one of the most important properties that can directly affect
Pavement quality, performance and serviceability. The lack of bonding between
bitumen and aggregates can cause stripping and significant reduction in Pavement’s
design Life. Different researchers have studied pavement performance using
overheated asphalt with asphalt becoming stiff with increase in temperature leading to
decreased penetration and increased viscosity due to vaporization of volatile oils. This
research aims to study relationship between temperature and bitumen binding
properties, change in degree of adhesion with increased temperature and effects when
bitumen is heated above its mixing temperature. ARL 60/70 Bitumen samples have
been heated to temperatures above its mixing temperature with various increments to
study the adhesive behavior. Samples were heated at 156oC (Virgin Bitumen), 160oC,
164oC, 168oC, 172oC. The Adhesive properties of bitumen have been evaluated on
loose Asphalt mix samples using rolling bottle test and Bitumen Bond Strength (BBS)
test. Results indicated that as temperature was increased after a certain temperature
bitumen-aggregate bond was affected adversely. Tests results have shown that
adhesion of bitumen with aggregate decreases as temperature is increased above mixing
temperature. This study suggests that ARL 60/70 bitumen should not be overheated at
temperature greater than 164oC to ensure proper bitumen-aggregate adhesion.

Keywords: Adhesion of asphalt binder, stripping, bond strength, overheated

bitumen,

iii
 UNDERTAKING

We certify that this research study “Effect of overheating on adhesion of Asphalt

Binder” is our own effort. This thesis has not been presented anywhere else. The
materials that were taken from other sources have been properly acknowledged and
cited.

Danish Abdullah 17-CE-60

Usama Mudassar 17-CE-84

iv
 ACKNOWLEDGEMENT

Starting with the name of ALLAH, the most Beneficent and the most Merciful.

All praises go to ALLAH who is the most Gracious, and Bountiful for providing us
the opportunity to study and do this work for the development of our country.
In Quran, He asks those who have knowledge and those who doesn’t, are they equal.
Allah has given us the most powerful gift of thinking and observing through which
humanity have strived so far.

Our Beloved Prophet Muhammad SAW, who bore hardships and difficulties to bring
us close to the ONE and ONLY GOD.

We thank our department’s faculty and chairman for their effort to make us able to
journey through our life and career.

We extend our heartiest gratitude to our project advisor, Prof. Dr. Naveed Ahmad for
the valuable endeavors, he rendered to us in the compilation of this exposition. we
express our sincere thanks to him, for he provided us a chance to work on this project,
which, we hope, shall prove to be valuable in our future career as well. Thanks to all
the faculty members of the Taxila Institute of Transportation Engineering and Lab
Supervisors for their continuous support, guidance, encouragement, and cooperation.

We pay our deepest gratitude with deepest sense of respect to our parents who
supported us. Their love and affection kept us steadfast and enabled us to attain targets
and goals of this arduous academic life.

v
 DEDICATION

To our Parents and Teachers (Spiritual Parents)

And
To our Family and Friends for their longing support and love

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 TABLE OF CONTENTS
ABSTRACT ............................................................................................................................. iii
UNDERTAKING .................................................................................................................... iv
ACKNOWLEDGEMENT ....................................................................................................... v
LIST OF FIGURES ................................................................................................................. x
LIST OF TABLES .................................................................................................................. xi
CHAPTER 1 ............................................................................................................................ 1
INTRODUCTION................................................................................................................... 1
1.1 Background ..................................................................................................................... 2
1.2 Problem Statement.......................................................................................................... 3
1.3 Objectives ........................................................................................................................ 4
1.4 Methodology .................................................................................................................... 4
1.4.1 Material ...................................................................................................................... 4
1.4.2 Durability analysis ..................................................................................................... 6
1.4.2.1 Tests used to measure/assess durability of asphalt mixes ....................................... 6
1.4.3 Tests selected for assessing adhesion......................................................................... 8
CHAPTER 2 .......................................................................................................................... 11
LITERATURE REVIEW .................................................................................................... 11
2.1 Transportation engineering ......................................................................................... 12
2.2 Highway/pavement Engineering.................................................................................. 13
2.3 Pavement Materials ...................................................................................................... 13
2.3.1 Soil ........................................................................................................................... 14
2.3.2 Aggregates ............................................................................................................. 15
2.3.2.1 Strength ............................................................................................................... 15
2.3.2.2 Hardness.............................................................................................................. 15
2.3.2.3 Toughness ........................................................................................................... 15
2.3.2.4 Durability ............................................................................................................ 15
2.3.2.5 Shape .................................................................................................................... 15
2.3.2.6 Adhesion with bitumen ........................................................................................ 15
2.3.3 Bitumen .................................................................................................................... 16
2.3.3.1 Workability: ........................................................................................................ 16
2.3.3.2 Durability ............................................................................................................ 16
2.3.3.3 Stability at high temperatures ............................................................................. 16
2.3.3.4 Ductility .............................................................................................................. 17

vii
 2.3.3.5 Adhesion to aggregates ....................................................................................... 17
2.4 Disbonding Mechanisms of Bitumen ......................................................................... 17
2.5 Adhesion of bitumen ..................................................................................................... 18
2.5.1 Active adhesion:.................................................................................................. 18
2.5.2 Passive Adhesion: ............................................................................................... 18
2.6 Adhesion Theories of Asphalt Mixtures...................................................................... 19
2.6.1 Mechanical adhesion Theory ................................................................................... 19
2.6.2 Chemical reaction theory ......................................................................................... 20
2.6.3 Theory of weak Boundary layer............................................................................... 20
2.6.4 Surface energy theory .............................................................................................. 20
2.6.5 Molecular orientation theory.................................................................................... 21
2.7 Factors affecting Bitumen-aggregate adhesion .......................................................... 21
2.8 Properties of Aggregates that affects adhesion .......................................................... 22
2.8.1 Effect of Mineralogy and chemical composition of aggregate on Adhesion ........... 22
2.8.2 Effect of surface texture of aggregate ...................................................................... 24
2.8.3 Effect of surface contaminants ................................................................................. 25
2.10 Properties of Bitumen that affects adhesion ............................................................. 26
2.11 Temperature sensitivity of Bitumen .......................................................................... 27
2.12 Effect of overheating on bitumen properties ............................................................ 28
2.13 Aging of Bitumen ........................................................................................................ 33
2.14 Aging Mechanism........................................................................................................ 34
2.14.1 Oxidative hardening ............................................................................................... 34
2.14.2 Loss of Volatiles .................................................................................................... 34
2.14.3 Steric Hardening .................................................................................................... 35
2.15 Types of Bitumen Aging ............................................................................................. 35
2.15.1 Short term Aging.................................................................................................... 35
2.15.2 Long term aging ..................................................................................................... 37
2.16 Effect of Aging process on properties of bitumen .................................................... 39
CHAPTER 3 .......................................................................................................................... 42
EXPERIMENTAL WORK .................................................................................................. 42
3.1 Experimental Work ...................................................................................................... 43
3.1.1 Temperature range ................................................................................................... 43
3.1.2 Number of Samples.................................................................................................. 43
3.1.3 Sample preparation for Bitumen Bond Strength test ............................................... 44

viii
 3.1.4 Sample Preparation for Rolling bottle test ............................................................... 44
3.1.5 Bitumen Bond strength test procedure ..................................................................... 45
3.1.6 Rolling bottle test procedure .................................................................................... 46
3.1.7 Flow Chart ............................................................................................................... 47
CHAPTER 4 .......................................................................................................................... 49
RESULTS AND DISCUSSIONS ......................................................................................... 49
4.1 Results ............................................................................................................................. 50
4.1.1 Bitumen Bond Strength Test ..................................................................................... 50
4.1.2 Rolling bottle test ...................................................................................................... 52
4.1.3 Comparison of loss in adhesion in both tests: ........................................................... 54
CHAPTER 5 .......................................................................................................................... 58
IMPACT OF THIS RESEARCH ........................................................................................ 58
5.1 Case Study ...................................................................................................................... 59
5.1.1 Cost effectiveness ..................................................................................................... 60
5.1.2 Resource Utilization.................................................................................................. 60
5.1.3 Ride quality ............................................................................................................... 60
CHAPTER 6 .......................................................................................................................... 61
CONCLUSIONS AND RECOMMENDATIONS .............................................................. 61
6.1 Conclusions ................................................................................................................. 62
6.2 Recommendations ....................................................................................................... 63

WORK CITED ...................................................................................................................... 64

Works Cited........................................................................................................................... 65

ANNEXURE A ...................................................................................................................... 70
ANNEXURE B ...................................................................................................................... 73

ix
 LIST OF FIGURES

Figure 1-1 Phase 1 of Methodology.............................................................................. 9

Figure 1-2 Phase 2 of Methodology............................................................................ 10
Figure 2-1 Different failure mechanisms between asphalt binder and aggregate
(Jakarni, 2012) ............................................................................................................ 18
Figure 2-2 Classification of aggregates based on their nature as hydrophobic or
hydrophilic .................................................................................................................. 22
Figure 2-3 interaction between bitumen and aggregate in the presence of water and
dust (AZKO Nobel, 2006) .......................................................................................... 25
Figure 2-4 Viscosity and penetration at 135 degrees (Nurfazilah, 2012) ................... 30
Figure 2-5 Average TODI for individual binder ( (sarnowski, et al., 2019)............... 31
Figure 2-6 Temperature and Penetration Value (baidya & singh, 2019) .................... 32
Figure 2-7 temperature and absolute viscosity (baidya & singh, 2019....................... 32
Figure 2-8 Temperature and Penetration value (baidya & singh, 2019)..................... 32
Figure 2-9 Relationship between softening point and mixing temperature (Shell
Bitumen Handbook) .................................................................................................... 36
Figure 2-10 Effect of bitumen thickness on aging index (Shell bitumen Handbook) 36
Figure 2-11 Aging of bitumen during mixing, storage and in service (Durability of
bitumen, The shell bitumen handbook) ...................................................................... 37
Figure 2-12 Viscosity at different oven heating duration (Dessouky, et al., 2011) .... 39
Figure 3-1 Rolling bottle test sample for 24 hours conditioning at room temperature
.................................................................................................................................... .45
Figure 3-2 Components of BBS Test .......................................................................... 46
Figure 3-3 Rolling Bottle Assembly ........................................................................... 47
Figure 3-4 Experimental work Flow Chart ................................................................. 48
Figure 4-1 Graph between Temperature and Pull off Tensile Strength ...................... 51
Figure 4-2 Bitumen Coverage after 6 hours of rolling time ....................................... 52
Figure 4-3 Bitumen Coverage after 24 hours of rolling time ..................................... 53
Figure 4-4 Bitumen Coverage after 48 hours of rolling time ..................................... 53
Figure 4-5 Bitumen Coverage after 72 hours ............................................................. 54
Figure 4-6 Percentage Loss in adhesion ..................................................................... 55
Figure 4-7 Loss per 4 Celsius ..................................................................................... 56
Figure A-1 failure surface for 156 degree temperature .............................................. 68
Figure A-2 Failure surface for 160 degree temperature.............................................. 68
Figure A-3 failure surface at 164 degree temperature ............................................... 68
Figure A-4 Failure surface at 168 degree temperature ............................................... 69
Figure A-5 Failure surface at 172 degree temperature ............................................... 69

x
 LIST OF TABLES

Table 1 Properties of ARL 60/70 bitumen .................................................................... 5

Table 2 Properties of Margalla Quary Aggregates ....................................................... 5
Table 3 Temperature and Penetration Index (Nurfazilah, 2012) ................................ 29
Table 4 Properties of Ages samples (The Shell Bitumen Handbook) ........................ 38
Table 5 Bitumen Bond strength Test results ............................................................... 50
Table 6 Percentage Loss in adhesion .......................................................................... 55
Table 7 Loss per 4° Celsius ........................................................................................ 56

xi
 CHAPTER 1

INTRODUCTION

1
1.1 Background

About 90% of the pavements in Pakistan and in the whole world are flexible pavements.
Flexible pavements consists of several layers such as subgrade, subbase, base course
and wearing course. Wearing course is made up of asphalt. Asphalt is a mixture of
aggregates, bitumen and filler. They are mixed in predetermined ratio to form a flexible
pavement. Construction of pavement consists of preparation of asphalt and transporting
them to place where it is laid and then compacted by means of roller and pneumatic
compactors. Some additives may also be added to increase the performance of asphalt
mixture. Different ratios of asphalt and aggregates result in different types of flexible
pavements. Although there are many factors on which performance of asphalt depends
yet adhesion is the most important factor. Adhesion can be defined as molecular force
of attraction in the area of contact between unlike bodies to hold them together. By
contrast, cohesion is the intermolecular force developed between the same body.
Adhesive is a substance which when applied to surface of materials, capable of joining
the materials and resists separation. The materials being joined are commonly known
as adherends or substrates. In case of asphalt, adhesion is usually referred to as amount
of energy that is required to break the bitumen-aggregate bond.

Adhesion is the most important property that must be ensured for proper functioning
of asphalt pavements and their durability because adhesion causes certain other
problems such as moisture infiltration and subgrade damage. There are several theories
that explain the phenomenon of bitumen-aggregate adhesion. The most important
factor which effect the adhesion is mixing temperature, viscosity of bitumen and
moisture penetration as indicated by present literature . Since bitumen is the visco-
elastic material, its properties change with the change in temperature. It softens when
heated and becomes stiff when cooled down. However, its an established fact in
literature that Overheating cause loss of volatile oils from bitumen and makes it stiff.
This affects the rheological properties of bitumen by increasing viscosity and
decreasing the penetration of bitumen.

2
1.2 Problem Statement

Adhesion of bitumen towards aggregates determine the quality of pavements and

performance under loading. Asphalt binder/Bitumen can be subjected to high
temperatures while manufacturing, mixing, transporting and laying. Sometimes due to
uncontrolled heating or longer mixing times and due to negligence of layman in
handling, bitumen gets overheated. These temperatures have negative effects on
binding strength of bitumen. Bitumen gets stiff on high temperatures due to
vaporization of volatile oils leading to brittle behaviour of Asphalt mixtures and
adhesion is also affected. The binding properties of bitumen are temperature dependent.
Lack of sufficient adhesive strength of bitumen with aggregates causes loss of
aggregates by stripping due to shear stress induced by traffic. Strong adhesion between
aggregates and bitumen also ensures water proofing and enable pavements to last
longer. Effect of aggregate minerology, surface texture of aggregates and surface
contaminants on adhesive bond between bitumen and aggregate exists in literature but
there are very limited studies that address the effect of bitumen properties on adhesion.
Despite the importance of adhesion, its relation with overheated bitumen does not exists
in literature and needs to be studied.

3
1.3 Objectives

1. To study the binding properties of 60/70 grade of bitumen when heated above
prescribed mixing temperature
2. To study the relationship between temperature and adhesion of bitumen in loose
asphalt mixture.
3. To find a temperature above which if bitumen is heated should not be used.

1.4 Methodology

A comprehensive literature review was done to have a background of research being

conducted and to decide the type of test that must be performed to assess the adhesion
of asphalt binder and aggregate and to get an overview that what relevant research has
already been done regarding adhesion of bitumen and overheating of bitumen. Studies
on material properties such as aggregate properties and bitumen properties were
performed based on previous literature. Selection of materials and test, preparation of
sample and testing procedures are summarized below.

1.4.1 Material

For this research, Aggregates from Margalla hills Quarry were used and Asphalt
binder/Bitumen produced by Attock Oil Refinery was used to form bituminous mix.
Bitumen of penetration grade of 60/70 was used. Properties of 60/70 PEN grade
bitumen of Attock Oil Refinery Limited (as provided by Attock Oil Refinery Limited)
are as follows:

4
 Table 1 Properties of ARL 60/70 bitumen

Test AASHTO
Test Description Units Max/MIn
Method M-20
Ductility @ 25oC cm D113 100 Minimum
o
Flash Point, COC C D92 232 Minimum
D5
Penetration @ 25oC 1/10 mm 60-70 -

Loss on Heating @
Wt% D6 1 Maximum
163oC
Penetration @ 25oC
%age D5 50 Minimum
(After loss on heating
Solubility in
Wt% IP47 99 Minimum
trichloroethylene
Ductility @ 25oC
(After Loss on cm D113 75 Minimum
Heating)
Properties of Margalla Aggregates are as follows (Munir, Abbas et al. 2017)

Table 2 Properties of Margalla Quary Aggregates

Properties of Margalla
Units Value
aggregates

Water Absorption % age 1.32

Specific gravity - 2.83

Bulk Density Kg/m3 1508

Voids % age 45.56

Impact Value % age 16.50

Crushing value % age 29.80

LA Abrasion value % age 17.2%

5
1.4.2 Durability analysis

Durability of asphalt is defined as its ability to resist traffic loads along with induced
environmental changes such as changes due to temperature and moisture. In asphalt
mix, bitumen and aggregates are mixed together to form uniform mix in which binder
coats the aggregates and form strong adhesive bond due to mechanical interlocking
between aggregate’s rough surfaces and binder. This adhesion is very important as it
determines the life of pavement and ride quality. When adhesion between bitumen and
aggregate is not strong enough to keep mix in place, stripping occurs and is defined as
removal of bitumen coating from aggregate surfaces due to repeated traffic loading and
moisture ingress. Adhesion between bitumen and aggregate can be weakened by many
factors such as improper mixing and improper use of binder content. Aging due to
oxidation of binder or loss of volatiles can also affect adhesion due to stiffness of
binder. It is very important to determine the bitumen-aggregate adhesion to properly
design the HMA and to ensure longer lasting pavements.

1.4.2.1 Tests used to measure/assess durability of asphalt mixes

Adhesion between aggregates and bitumen is tested in terms of the stripping potential
of aggregates. Most common tests that are used to assess the affinity/adhesive strength
of asphalt binder with aggregate have been standardized by part 11 of BS EN 12697-
11 : 2005. Following are the most common tests that can be performed to assess
adhesion (Whiteoak 2003)

• Rolling Bottle test

• Static Water immersion Tests
• Chemical Immersion Tests
• Pull off test

1.4.2.1.1 Rolling bottle test

British standard has provided specifications to perform rolling bottle test on loose
asphalt mix. Bitumen’s susceptibility to stripping is and indirect method to determine
the affinity of bitumen to various aggregates or affinity of various binders to

6
aggregates. This test can also be used to determine the effect of adhesion promoters
and also determines the moisture damage. Rolling bottle test is simple to perform but
is a subjective test and is considered appropriate for ordinary testing. It is not
recommended for aggregates that are highly abrasive in nature. The process involves
the mechanical stirring of aggregates in presence of water and then determining the
degree of bitumen coverage after 6, 24, 48 and 72 hours of rolling time. Degree of
bitumen coverage is determined visually, taking average of the readings of two
observers.

1.4.2.1.2 Static Water immersion test

This is considered as the simplest test to assess the affinity of aggregates. It requires
loose mix to be immersed in water for specific period at 25oC and the degree of bitumen
coverage is estimated visually. The only problem with this method is its subjective
nature and poor reproducibility. However, this drawback can be somehow overcome
by visual observation taken by experienced person. Occasionally, aggregates with poor
static immersion test may perform better in service.

1.4.2.1.3 Chemical Immersion tests

This method involves testing the bitumen coated aggregates by boiling in water in
which solution of sodium carbonate is also added. after letting aggregates in solution
for sometime, stripping occurs and the solution concentration in which stripping is
observed first is considered as the measure of adhesive strength of bitumen towards
aggregates. The artificial conditions of test may not be a true representative of asphalt
performance on roads

1.4.2.1.4 Pull-off tests

There are several pull-off tests that can be used to assess the adhesion potential of
bitumen such as Instron pull off, Limpet Pull off and Pneumatic Adhesion tensile
Testing (PATTI). In instron pull off test, Instron tensile apparatus is used to extract the
specimens of aggregates from bitumen containers under controlled conditions. In
limpet pull off test, limpet apparatus is used to determine the bond strength between
aggregate of surface and those aggregate that are underlying the surface dressing.

7
Bitumen Bond strength Test Uses PATTI to determine the strength needed to detach
the bitumen from aggregate surfaces. It is simple test and was originally developed to
use in paint industry. BBS test procedure that is now a days used in Bitumen was
developed at university of Wisconsin-Madison in collaboration of University of
Ancona and university of Stellenbosch. It is used to quantify the adhesive bond
between aggregates and binder and also used to study the moisture damage and
conditioning of temperature and waster conditioning.

1.4.3 Tests selected for assessing adhesion

We selected following two tests from above mentioned test to assess adhesion

• Rolling Bottle Test

• Bitumen Bond Strength Test

These two testing techniques were selected based on the simplicity, practicality and
ease of sample preparation.

A research was carried out in Germany to determine the suitability of adhesion tests
and to determine the best test among all tests that are present in European standard.
Both merits and demerits of these tests were studied and found out that among all
adhesion tests, Rolling Bottle test is considered as the most simple yet effective test
because aggregates are continuously subjected to water and mechanical action that is
closely related to field conditions. The other tests such as static water and boiling water
did not give accurate results (Renken, et al., 2010). However, static method can be used
by some modifications regarding mixing temperature and water conditioning
temperature as stated by (Hugener, et al., 2012)

BBS test has been selected because of its simplicity and accuracy. The pullout tensile
strength and failure surface mode are used to characterize the bond strength between
aggregates and bitumen.

Our methodology is divided into two phases. Phase 1 deals with the procurement of
material and study of present literature including testing techniques while 2nd phase
involved testing of loose mix samples using selected tests and analysis of results. After

8
 the selection of aggregate and bitumen and testing techniques, a comprehensive
experimental plan was drafted to proceed the research and after that results were then
evaluated and conclusions were drawn. Following flow chart summarizes our
methodology that was adopted to accomplish our goals.

Adhesion of bitumen

Literature review

Overheating and aging effects

Phase 1

ARL 60/70 PEN Bitumen

Material selection

Margalla aggregates quary

Rolling bottle test (BS EN 12697-

11:2005)
Selection of testing
techniques
Bitumen Bond Strength test
(AASHTO T 361)

Figure 1-1 Phase 1 of Methodology

9
 Sample preparation Sample Testing

Visual Observations
Phase 2

Observations and analysis of

results
Calculations and Graphs

Recommendations and
Conclusions

Figure 1-2 Phase 2 of Methodology

10
 CHAPTER 2

LITERATURE REVIEW

11
2.1 Transportation engineering

Transportation Engineering is a branch of civil engineering that is mainly involved in

design, maintenance, planning and construction of roads, railways, harbors, airports,
traffic control systems, bridges etc. They carefully examine the demand and supply
situation in their field. For a transportation engineer, demand is the amount of traffic
that is expected to use the particular facility such as number of people, cars, trucks,
buses, ships, airplanes etc. He/she then decide the size and quality of infrastructure
components to meets the required demands. For example, considering an example of a
road, if road is between two major cities (Interstate highway), it must be of high quality
with wider and more number of lanes, constructed with good quality practices and
materials, as compared to roads within a city. Same is the case with the airports,
Transportation engineer will decide the number of runways, runway length and width
based on the type of aircraft using the facility. For wide body aircrafts, long and wider
runways are required as compared to small narrow body aircrafts.

Transportation Engineers utilize the most recent developments in the field of

transportation and uses them to develop the most systematic and sophisticated transport
systems for various localities. They combine the skills of inventiveness with the science
of construction to come up with innovative new systems and solutions.
The main components of transportation engineering includes:

• Highway/Pavement Engineering
• Highway maintenance
• Traffic Engineering and control systems.
• Public transit systems
• Airport Engineering
• Bridges
• Waterways
• Seaports

12
2.2 Highway/pavement Engineering

Highway Engineering is an engineering discipline origination from transportation

engineering that includes, design, planning, construction, operations and maintenance
of roads, and highway bridges to ensure safe and efficient transportation of goods and
people. Highway engineer takes into consideration the expected future traffic flow for:

• Designing intersections and large highway interchanges

• Horizontal and vertical alignment
• Selection of pavement materials
• Structural design of pavement thickness to ensure long lasting pavement.

He is also responsible for pavement maintenance and rehabilitation of damaged

pavements.

2.3 Pavement Materials

Pavements are combination of different types of materials. Properties of these

materials, their interaction with each other, determine the performance related
properties of resulting pavements. These are mainly loose materials like soils and
aggregates and binder materials that binds the loose material together. They may also
contain some miscellaneous materials or admixtures to improve the load carrying
capacity and serviceability of pavements. For flexible pavement, binder is usually
Bitumen and for rigid pavements, hydraulically bound material is used with cement as
binder.

Soil serves as foundation of pavement that bears all loads coming from pavement
layers. Soil is the main constituent material in case of highway constructed on
embankment. Soil is well compacted before road construction to improve is bearing
capacity. Mineral loose aggregates obtained from natural rocks and mountains form the
major constituents of base and subbase of most of the highways. Binders such as
bitumen and cement are used for top layers that are in direct contact with vehicle.
Bitumen, also termed as Asphalt binder, is mixed with appropriated aggregates in

13
proper proportion and is used as wearing course in Flexible asphalt pavement. Cement
mixed with aggregates are used in heavy duty pavements called Rigid Pavements.
Sometimes both hydraulically bound material and bitumen bound material is used in
same pavement, termed as composite pavements.

2.3.1 Soil

Soil is a natural material, mainly derived from disintegration and weathering of rocks.
The soil that supports the pavement is call subgrade soil. Soil is present in its natural
state i.e loose state. It requires proper compaction to make it suitable for use as a
subgrade.

Desired properties of subgrade soil are as follows:

• Stability
• Ease of compaction
• Resistant to volume changes
• It Should be stable under adverse weather conditions and ground water
fluctuations
• It should have good drainage capabilities.
• It should have high resilient modulous

Properties of subgrade soil are highly involved in design of pavement thicknesses. The
main purpose of subgrade is to support the pavement to perform well during its design
life and for this function to be fulfilled, subgrade properties must be evaluated for its
stability and strength under applied loadings. These properties can be evaluated using
different test on subgrade soil. Following test are used to evaluate subgrade properties:

• Shear tests
• Penetration tests
• California bearing ratio test (CBR)
• Plate load test

14
2.3.2 Aggregates

Stone aggregates are the most important material that is used in the construction of
pavements. These are derived from rocks by breaking and crushing the rocks to specific
required sizes. They are used for bituminous wearing course, granular base course and
subbase. Determination of aggregate properties, their types, strength parameters and
capability of drainage is of utmost importance for highway engineer in designing long
lasting pavements. Following are the desirable properties of aggregates to be used in
highway pavements.

2.3.2.1 Strength
Aggregate must have resistance to crushing under load especially in top layers
such as wearing course.

2.3.2.2 Hardness
Aggregates that are used in pavements must have abrasion resistance. The
rubbing action of tyre must be resisted efficiently.

2.3.2.3 Toughness
Aggregates, in addition to hardness and strength, must have sufficient
toughness to resist the impact load of trucks and heavy vehicles which are
applied during acceleration and deceleration.

2.3.2.4 Durability
Aggregates should have good resistance to weathering due to forces of nature.
This property is called soundness

2.3.2.5 Shape
Aggregate must be of proper shape and size, a good balance between flakiness
and elongation, too flaky or too elongated particles give less pavement strength
To ensure good interlocking, aggregates must be preferably cubical or angular.

2.3.2.6 Adhesion with bitumen

Aggregates should have greater affinity towards bitumen and should have less
affinity towards water to prevent moisture damage. It should be porous enough
so that bitumen gets absorbed in its pores and form strong enough bond to
prevent water damage. Thus aggregate should be hydrophobic.

15
2.3.3 Bitumen

Bitumen has been in use as bonding and water proofing material since centuries. Its use
in pavement emerged in 19th century. As demand for petroleum increased, refining of
crude oil increased, the residue that is left behind called bitumen and tar found
increased use in pavements that provide excellent ride quality due to resulting smooth
surface. American Society for Testing materials (ASTM) defined bitumen as:

“Bitumen is a hydrocarbon material of natural or pyrogenous origin, which is in a

gaseous, liquid, semi solid or solid state that is completely soluble in carbon
disulphide”.

Bitumen has following important properties:

• It is predominantly hydrocarbons
• It gets soft when heated and becomes hard when cooled down
• It has no affinity for water i.e highly impermeable
• It is not chemically active and does not react with most acids, alkalis and salts
• Although bitumen is usually hydrophobic, it can be made hydrophilic by
addition of surface active agents.

For a bitumen to be used in roads, following properties are desired:

2.3.3.1 Workability:
Bitumen should be in fluid form when mixing with aggregates so that
aggregates are fully coated and bitumen gets into pores to form a strong bond
with aggregate surface.

2.3.3.2 Durability
Properties of bitumen should not or change to a very limited extent in varying
temperatures

2.3.3.3 Stability at high temperatures

Bitumen is a result of refining of crude oil so it has some petroleum constituents
in it. These are volatile in nature. So when bitumen exposed to high
temperatures during manufacturing of asphalt and mixing, these volatile oils

16
 should not evaporate excessively to ensure durability and ductile behavior of
bitumen.

2.3.3.4 Ductility
Bitumen should have sufficient ductility. It should be flexible to deform under
load and then return back to its original state after removal of load. But it should
not be so much flexible that leads to rutting of asphalt pavements.

2.3.3.5 Adhesion to aggregates

Bitumen should exhibit good affinity towards aggregates surface and should
resist stripping in the presence of water.

2.4 Disbonding Mechanisms of Bitumen

According to The Shell Bitumen Handbook, there are mainly two types of disbonding
mechanisms of bitumen,

• Adhesive
• Cohesive.

It depends on state of aggregate that which type of failure will occur. If aggregate is
clean and dry, bituminous mixture will be impermeable and failure type will be
primarily cohesive. Whereas, if aggregate is wet or in the presence of water or water
vapours, failure will be mainly due to adhesion loss between bitumen and aggregate.
Several other mechanisms are also possible such as:

• Displacement
• Detachment
• Blistering and peeling
• Film rupture
• Chemical disbonding

17
2.5 Adhesion of bitumen

Adhesion is successfully defined by American Society for Testing Materials (ASTM

D907) as

“A state by which two dissimilar surfaces are held together by interface forces which
can be either valence force or interlocking forces or both”

(Pasadin & Perez, 2015) defined two types of adhesion in case of bituminous
pavements: Active adhesion and passive adhesion.

2.5.1 Active adhesion:

The ability of asphalt binder to completely coat the aggregate surface while
mixing and manufacturing of asphalt concrete in Hot Mix Asphalt Plants is
called active adhesion.

2.5.2 Passive Adhesion:

Passive adhesion is adhesion of binder during pavement service life. it is ability
of binder to resist stripping and displacement from aggregate surface under the
action of water and repeated traffic loading.

Bitumen and stone aggregates are main components of Asphalt. Their properties,
chemical composition and physical characteristics directly affects the performance of
asphalt pavements (Grenfell, et al., 2014).

Figure 2-1 Different failure mechanisms between asphalt binder and aggregate
(Jakarni, 2012)

18
Adhesion is one of the major properties of bitumen. Strong bonding between bitumen
and aggregates is crucial to have high performance pavements. Lack of affinity between
bitumen and aggregate leads to moisture damage in asphalt pavements that significantly
reduces the life of asphalt pavement (Grenfell, et al., 2014). How strong the bitumen-
aggregate bond is and how resistant a bitumen is against stripping in the presence of
water depends largely on chemical characteristics and properties of bitumen, internal
structure of bitumen and chemical composition of aggregates. Although failures related
to adhesion of bitumen are very rare but failures can be considerable expensive, when
they occur. Thus, it is very important to ensure adhesion of bitumen with aggregates.

2.6 Adhesion Theories of Asphalt Mixtures

Till today, various adhesion theories have been in use to describe Asphalt binder-
aggregate adhesion such as Mechanical adhesion, Chemical reaction, Weak Boundary,
Thermodynamic, Surface energy and Molecular orientation Theories. These Theories,
however, can only explain some aspects of adhesion between bitumen and aggregate
and still cannot completely explain the mechanism. (Jakarni, 2012)

2.6.1 Mechanical adhesion Theory

Physical properties of stone aggregates such as, shape, porosity, angularity, surface
texture, particle size and surface areas effect the adhesive bond between aggregates and
bitumen according to this theory. This theory shows that adhesive bond is developed
due to interlocking between bitumen and aggregate surface. Aggregates with porous
and rough surfaces can improve interlocking between asphalt binder and aggregate and
can form strong adhesive bond. Bitumen penetrates into aggregate pores and surface
roughness, irregularities and cavities, it then hardens and mechanically grips the surface
and forms a bond. (A.W, et al., January 2005).

19
2.6.2 Chemical reaction theory

Chemical reaction theory explain why extent of adhesion between bitumen and
aggregate is different. Aggregates are either hydrophilic or hydrophobic based on their
surface roughness, chemical composition, porosity and pore size. Aggregates that are
more attracted towards water tends to show stripping to much higher degree than
hydrophobic aggregates. Acidic compounds in bitumen and alkaline nature of
aggregates tend to form much stronger bond than a bond between acidic bitumen and
acidic aggregate. This shows that pH of aggregate surface greatly influence the strength
of adhesive bond between asphalt binder and aggregate. (Wenyi , et al., 2020).

2.6.3 Theory of weak Boundary layer

This theory states that failure can be either adhesive or in substrate due to presence of
low adhesion/cohesion region. Contaminants on aggregate surface, dust and some
organics material are cause of weak boundary layer (arno, 2005) . He further stated that
dust particles present on aggregate surface can prevent proper contact between surface
and bitumen.

2.6.4 Surface energy theory

For an effective bond formation between bitumen and aggregate, bitumen should coat
aggregate as completely as possible. The ability of bitumen to coat the aggregate i.e
wetability of bitumen can be explained using surface energy theory (Jakarni, 2012).
Surface energy is defined as energy required to form a new surface between aggregate
and bitumen. The adhesion tension formed when bitumen is brought in contact with
aggregates is less than the adhesion tension of aggregate and water. So there are greater
tendency for bitumen to get stripped off in presence of water. Adhesion tension
depends upon aggregate types, aggregate roughness and nature of bitumen. (Jakarni,
2012). (Anon., 2009)

20
2.6.5 Molecular orientation theory

This theory explain that when bitumen is mixed with aggregates and is in contact with
aggregate surface, bitumen molecules tend to rearrange themselves in order to
maximize the contact area between binder and aggregate and to satisfy the energy
demands of aggregate surfaces. (Hicks & R.G, 1991) stated

“Molecules of water are dipolar. Molecules of bitumen are generally non-polar,

although some components are polar. Consequently Molecules of water being more
polar, may more satisfy the energy demand of aggregate surfaces”.

It’s a common understanding that water molecules are more polar than bitumen thus
Depending upon composition of aggregates, water may satisfy energy demands more
than bitumen and potentially cause stripping of bitumen from aggregates. This may
explain why bitumen is stripped off from aggregate surface in presence of water.

2.7 Factors affecting Bitumen-aggregate adhesion

Asphalt mixture consist of coarse aggregates, fine aggregates and filler material.
Durability of asphalt pavement is based on the cohesion and adhesion of asphalt binder.
The adhesive bond of bitumen-aggregate is a complex phenomenon to analyse due to
various factors involved in its development. Adhesion depends upon Bitumen
Properties, Properties of aggregates, external factors. Aggregate properties such as,
dust, surface texture, minerology, porosity, surface area, absorption, shape etc.
influence the adhesive bond between aggregates and bitumen. Similarly, bitumen
properties such as, chemical composition, polarity, internal structure etc. greatly affect
adhesion. Some external factors such as, rain, environmental temperature, pH,
Humidity, Moisture, Traffic also affect adhesion of bitumen with aggregate.

Physical-chemical properties of aggregates such as surface chemistry, morphology tend

to affect bitumen interaction with aggregates to much higher degree than bitumen
chemistry (cui, et al., 2014).

21
2.8 Properties of Aggregates that affects adhesion

It is the nature and properties of aggregates that are dominant factors among all factors
affecting adhesion. Various studies have found that stripping in asphalt mixture is
related mineralogical composition and surface texture and roughness of aggregates.
The aggregates are comprised of more than one type of mineral that has specific atomic
structure and arrangement. Their atomic arrangement is such that each atom is bounded
with other atom in three dimensional structure by electrostatic forces (cui, et al., 2014).

2.8.1 Effect of Mineralogy and chemical composition of aggregate on Adhesion

Rocks that are crushed to get road construction aggregates are mostly “Silicate
Minerals” which have compounds of silicon and “Calcite minerals” (Twagirimana,
2014).

Figure 2-2 Classification of aggregates based on their nature as

hydrophobic or hydrophilic
(Airey, et al., 2008) when assessed water damage mechanism in asphalt found that less
striping of bitumen occurred when basic aggregates was used such as limestone than
when acidic aggregates such as granite was used to form bituminous mix. They
concluded that limestone is more resistant to stripping due to its positive charge that
forms strong bond between bitumen and aggregate. They termed “Limestone” to be
“hydrophobic” and suggested that silica usually reduces the bond strength as limestone
has less silica as compared to Granite, it shows better water ingress resistance. similar
results were shown by (Ammara, et al., 2018) in which limestone showed better

22
adhesion towards bitumen because of its basic nature. Another study using basalt
aggregates also concluded that mineralogical composition of aggregates significantly
affects adhesive bond. (Zhang, et al., 2015) also examined effects of minerology of
aggregates on aggregate-bitumen bonds using limestone and granite aggregates and
two bitumen grades 40/60 and 70/100. They performed peel test and Pneumatic
Adhesion Tensile Test to study the stripping behaviour and found that effect of bitumen
properties on adhesion is lower than that of aggregate properties. Their results
supported the literature that shows aggregate materials that affect adhesion in a
negative way are siliceous compounds with addition of anorthite and clay in the list of
detrimental aggregate materials. Another study conducted by (Yin, et al., 2017) in
which main composition of limestone and granite aggregate were studied using X-Ray
Diffraction and Dynamic Shear Rheometer DSR test was performed to study
rheological properties. They found that limestone-bitumen adhesion is over 10%
stronger than granite-bitumen adhesion without abrasion when same aggregates were
subjected to 1000 abrasion cycles, they concluded that adhesion of limestone-bitumen
was much stronger than granite-bitumen but this time it was only 6% stronger. (L.O,
et al., 2019) studies the effect of aggregate morphological properties that effect
stripping behaviour. They used two aggregate sources (Granitic and Phonolitic) and
two binders, one neat and other modified with anti stripping agent. Static water storage
test and digital image processing was used to evaluate test results. Results indicated
that granitic aggregates performed better in terms of adhesiveness when mixed with
both neat and modified bitumen. They further added grounded plastic bags into the
mixture and found better adhesion as compared to control mixture. They concluded
that aggregates angularity, texture, porosity do not appear to effect aggregate binder
adhesion to such extent that aggregate internal composition effects such as related by
Fe2O3 and CaO. (Cala, et al., 2019) also demonstrated effect of mineralogical
composition of aggregates on adhesion of bitumen and tested adhesion of aggregates
derived from mafic rocks and Felsic rocks and demonstrated that mafic rocks show
better aggregate-bitumen bond strength and are less susceptible to moisture damage as
that of Felsic rocks. Shuang Cui and Bamber R.K supported the literature that basic
aggregates are hydrophobic but they observed that although limestone and marble both

23
are basic but marble has better adhesion and moisture resistance due to its less porosity
and more rough texture (Cui, et al., 2014)

2.8.2 Effect of surface texture of aggregate

Several other factors also affect adhesion such as surface texture and presence of dust
on aggregate particles. Coarse mineral rocks such as feldspar produce many flat and
smooth surfaces when crushed thus they show less adhesion as compared to fine
grained rocks that produce irregular surface when crushed.

Physical characteristics of aggregates surface have been shown by studies to affect

stripping behavior significantly. Surface texture of aggregates affect the bitumen
coverage on aggregates and easiness of coating. When aggregates are mixed with
bitumen, bitumen tends to penetrate deep into fissures and pores that it is felt that a
strong bond is formed between aggregate and bitumen due to penetration of binder into
pores and resulting mechanical interlocking. Research shows that when aggregate is
crushed from rocks and immediately used in asphalt mix exhibits poor resistance to
stripping than when aggregate is stockpiled for sometime and then used later (tarrer &
Wagh, 1991). Pocius (1997) evaluated the effect of surface roughness on adhesion and
stated that surface roughness prevents abrupt plan stress transfer. Therefore, due to
adhesive nature, rough surface of aggregates may promote dissipation of energy around
the crack. He also stated that by increasing contact area increases the adhesion of
bitumen. In a study, involving different aggregate (with different surface characteristics
morphology such as smooth and fractured) and binder combinations and evaluation of
adhesion strength using Bitumen Bond strength test. Results showed that fractured
surface affected aggregate-bitumen bond in a negative way than smooth surface
(stander, et al., 2011)

(tarrer & Wagh, 1991) stated that smooth aggregate surface is easier to wet than rough
surface . Further, aggregates that are dry shows better adherence to bitumen than wet
aggregates. When aggregates are heated to such high temperature that absorbed water
films are evaporated, this reduces interfacial tension between aggregate and bitumen
and thus reduces the tendency of aggregate to strip off (Bowen, et al., 2020). If

24
aggregate has unbalanced surface charge then it possess surface energy, if such surface
is coated with substance that has opposite charge as that of aggregate surface, it will
form strong bond (Zhang, et al., 2015).

2.8.3 Effect of surface contaminants

Dust on aggregate surface is another factor that affects coverage of bitumen. It

adversely affects HMA performance and can lead to deterioration of pavements.
Studies show that dust on aggregates can cause blistering and pits that cause stripping
of bitumen from aggregate surface and promotes water ingress. It was observed that
presence of dust on aggregate particles also prevent effective adhesion. Dust has
tendency to trap air and prevent proper adhesive bond formation. Following image
illustrates how dust and damp aggregates affects bitumen-aggregate

Figure 2-3 interaction between bitumen and aggregate in the

presence of water and dust (AZKO Nobel, 2006)

(Akbulut, et al., 2013) performed test on aggregate with different dust contents. They
generated artificial dust by using cylindrical drum equipment that simulate the dust
generation in field i.e due to handling. Aggregates were grouped into three categories
based on dust content with no, medium and high dust content. Results indicated that
Marshall Stability was lowest for aggregate mix with high dust content and also.
Marshall immersion test indicated that with increase in dust, moisture ingress resistance

25
decreases this is due to the fact that aggregates are not coated completely due to
presence of dust.

2.9 Effect of additives on Adhesion of Bitumen-Aggregate system

Additives are either natural or chemical based that are used to improve several
performance related properties of Asphalt mixtures. They tend to promote adhesion
between bitumen and aggregate. Jie Ji and Hua Yao evaluated the effect of organic
additives on adhesion of aggregate asphalt interface using surface free energy method
and showed that when surface free energy ratio increases, the adhesion of asphalt
aggregate mixture modified with organic additives decreases. Organic additives have
been found to promote adhesion in dry conditions because of their hydrophobic nature
while in wet condition adhesion decreases (Ji, et al., 2017). The use of mineral filler
improves the passive adhesion of bitumen thus increasing the durability. Fillers such
as Portland cement and CEM II/B-M 32.5 N Tend to improve bitumen coverage
however natural fillers did not show active adhesion imporvemant than commercial
products (Pasadin & Perez, 2015).

2.10 Properties of Bitumen that affects adhesion

By far, it has been established that bitumen-aggregate interaction is mainly influenced

by properties of aggregates and properties of bitumen has very little influence on
adhesion. Following are some properties of bitumen that play an important role in
adhesion of asphalt

• Composition and source of origin of bitumen

• Weathering effects
• Oxidative effects and curing time
• Electrical polarity
• Viscosity
• Rheological properties of bitumen

Perhaps, viscosity and surface tension are the most important parameters related to
bitumen that affects adhesion. The amount of bitumen absorbed into pores to create

26
strong bond depends upon these to parameters. Heating of bitumen makes it soft and
enables it to completely coat the aggregate surface thus forming adhesive bond. Extent
of absorption of bitumen was observed and found that strong bond is formed at
aggregate interface with layer thickness of 180 Amstron (anonymous, n.d.). Not much
literature is available on the properties of bitumen that affects adhesion. However
(torregrosa, et al., 2007) also stated that viscosity of bitumen and temperature at which
bitumen is mixed significantly affects the adhesion process.

2.11 Temperature sensitivity of Bitumen

Bitumen is an inexpensive material is widely used in pavements throughout the world.

The term “Temperature sensitivity” refers to the fact that properties of bitumen such as
viscosity and flow changes with the change in temperature. Bitumen is a hydrocarbon
mostly composed of long chains of carbon and is viscoelastic material. Its state changes
with temperatures as follows:

When temperature increases

Solid → semisolid → liquid

When temperature is reduced

Liquid → semisolid → solid

Bitumen tends to become soft when temperature is increased and can cause
permanent deformation in Pavements. Also, when temperature is reduced bitumen
lose its elasticity and becomes brittle leading to cracks.

When temperature is increased and increased with constant rate and there is little or no
change in rheological properties of bitumen that shows that this bitumen is less
sensitive to temperature instead when temperature is increased and viscosity rapidly
changes that shows high temperature sensitivity of bitumen.

If viscosity of bitumen is very high, it will be very difficult for bitumen to completely
and effectively coat the aggregates also, if viscosity is very low, drainage of binder may

27
occur during handling that also affects wettability of aggregates (Nurfazilah, 2012),
thus bitumen has to be sufficiently viscous to avoid both scenarios.

Bitumen properties doesn’t significantly change within a certain temperature range

called mixing temperature. When bitumen is handled at or below the mixing
temperature then its rheological properties are not affected and is suitable to make
asphalt mixes. But when temperature is increased above mixing temperature i.e when
bitumen is overheated, its rheological properties significantly change and aging process
begins. Several researchers have worked to determine the overheating effects on
bitumen properties. Most of them targeted the rheological properties and not focused
on the absorption of bitumen into aggregate pores and adhesion of bitumen towards
aggregate.

2.12 Effect of overheating on bitumen properties

During mixing and preparation of asphalt mix, bitumen can accidently or due to
negligence of workers, might get overheated that may cause hardening of bitumen at
early stages. This may lead to increased viscosity and aging.

A study conducted by (Lolly, 2013) to evaluate the aging effect of bitumen due to
elevated temperature The study involved two different performance graded bitumen
(PG 64-22 and PG 76-16) and two elevated temperature and time the one being
standard temperature and time and the other was elevated temperature and time and
the their viscosities were measured. Results indicated that for both cases of elevated
temperature and elevated exposure time, there was an increase in viscosity due to loss
of volatile oils and leaving behind stiff matter. Binders were heated and mixed at
temperature 25oF above standard mixing temperature and exposure time was elevated
upto 4 hours. Results showed that elevating the temperature and exposure time,
stiffness of samples were increased. Dynamic modulus for design remained unchanged
during 2 hours of aging time but Appreciable changes in dynamic modulus occurred
during first four hours of aging leading to increased viscosity. Furthermore, on
increasing STA time from 85 minutes to 175 minutes binder’s viscosity increased by
twice.

28
Another study conducted by (Nurfazilah, 2012) involving overheated bitumen to
prepare HMA. He performed penetration test, softening point test, rotational
viscometer, and Marshall mix design to determine the change in rheological properties
of bitumen when overheated. 60/70 PEN grade bitumen was overheated at 175oC,
185oC, 195oC, 205oC, 215oC and 225oC for 3 hours in a preheated oven. Results
indicated that the overheated bitumen affects the HMA properties of mix to significant
extent. Bitumen can oxidize and gets stiff due to very high temperature. This fact was
supported by the research conducted by (Nurfazilah, 2012) in which Penetration index
value decreased as heating temperature of bitumen is increased, followed by increased
viscosity and decrease in needle penetration. Softening point also got elevated.

Also, penetration index has also been decreased as shown by following table

Table 3 Temperature and Penetration Index (Nurfazilah, 2012)

Temperature oC Penetration Index (PI)

165 -1.50
175 -1.25
185 -1
195 -1.25
205 -1.5
215 -1.25
225 -2

Figure mentioned below shows the relation between viscosity and penetration of
overheated bitumen. Its R2 value is 0.858 which indicates that good correlation exists
between penetration and viscosity which is obvious as supported by literature that
viscosity increases and penetration decreases when binder is overheated due to
initiation of aging process.

29
 Figure 2-4 Viscosity and penetration at 135 degrees
(Nurfazilah, 2012)

The test gave maximum limit temperature of 189oC before 60/70 starts to lose its
rheological properties. Since overheated bitumen is harder than virgin/neat bitumen, so
HMA produced by using overheated bitumen will have higher stability as compared to
stability value of virgin bitumen. Thus, it can be expected to be less susceptible to
rutting.

(sarnowski, et al., 2019) also studied the influence of overheating on bitumen

properties. They performed analysis on virgin bitumen and SBS modified bitumen
heated at 200, 250, 300oC for 1 hour. They developed a degradation index which was
used to characterize the properties of bitumen based on temperature increments. Angle
of inclination of ODI line is zero when bitumen is resistant to overheating and is infinity
when bitumen is highly sensitive to overheating. When ODI value changes from
negative to positive or vice versa it crosses the ODI zero that enables the person to read
TODI. They determined the limit temperature for binder by taking average of TODI for
softening, penetration and viscosity. Results indicated that lower overheating
sensitivity was exhibited by 50/70 bitumen while highest sensitivity was exhibited by
PMBs.

Results concluded that maximum resistance to overheating was exhibited by bitumen

35/50 i.e its limit temperature is 235oC it was followed by 50/70 and 20/30with limit

30
temperatures of 229oC and 227oC respectively. Lowest limit temperature was showed
by SBS modified bitumen as shown by following figure.

Figure 2-5 Average TODI for individual binder (

(sarnowski, et al., 2019)

A study conducted to determine the effects of overheated binder on binder content and
marshal properties of the mix by (baidya & singh, 2019) in which bitumen was heated
in oven at 5 temperatures i.e 185, 195, 205, 215 and 225 degrees for 3-4 hours and
properties of bitumen and then asphalt mix using that overheated bitumen was
determined. Their results supported the existing literature as of (Nurfazilah, 2012) that
penetration value decreased with increase in temperature (figure 7) and also viscosity
is increased (figure 8) followed by increase in the softening point (figure 9) due to aging
process that was initiated by overheating of bitumen. Results also indicated PI value of
bitumen which must be between -2 and +2. Smaller PI value indicated brittle bitumen
and higher PI value indicated softer or ductile bitumen. Results indicate that PI value
goes on decreasing but with and increase at temperature 215oC beyond which bitumen
became brittle and asphalt may become susceptible to cracking

31
 Figure 2-6 Temperature and Penetration value (baidya & singh, 2019)

Figure 2-7 temperature and absolute viscosity (baidya & singh, 2019

Figure 2-8 Temperature and Penetration Value (baidya & singh, 2019)

32
2.13 Aging of Bitumen

Bitumen is greatly affected by the presence of UV rays, oxygen and temperature

variation. According to Shell Bitumen handbook, These factors tend to harden the
bitumen that results in elevation of softening point, decrease in needle penetration and
increase of the penetration index Increase in softening point and decrease in penetration
indicate that bitumen has now become stiff and viscosity is increased.

Aging also occurs when bitumen is overheated above its mixing temperature. When
bitumen is heated above its mixing temperature it can take effect of temperature change
upto 4 to 5oC above its mixing temperature after that aging of bitumen starts and
bitumen gets progressively harder and stiff with is viscosity greater than neat bitumen
and less penetration with elevated softening point temperature. This aging is perhaps
due to evaporation of volatile oils that constitute bitumen and stiff matter is left behind.

Aging can occur either during mixing and production of asphalt or during the service
life of the pavement. There are several factors that have been identified by The Shell
Bitumen Handbook that affect the asphalt aging

• Production Plant type

• Mixing temperature
• Silo storage time
• Field conditions such as temperature, UV Rays and rainfall
• Aggregate gradation
• Void content
• Thickness of asphalt content

33
2.14 Aging Mechanism

Aging can occur through various modes and mechanisms. Shell Bitumen Handbook
has outlined various aging mechanisms of bitumen, these are as follows (Read &
whiteoak, 2003)

2.14.1 Oxidative hardening

When bitumen or asphalt mixture comes in contact with atmosphere, oxygen present
in atmosphere reacts with bitumen to form polar hydroxyl and carboxylic groups that
results in complex and larger molecule formation that leads to decreased flexibility and
increased hardness. Degree to which bitumen hardens by oxidation process depends
upon

• Temperature at which bitumen came into contact with atmospheric oxygen

• Exposure time of bitumen with atmospheric oxygen
• Thickness of bitumen film during contact with atmospheric oxygen

According to shell bitumen handbook, it has been observed that rate of oxidation id
greatly influenced by temperature so much so that for each 10oC increase in
temperature above 100oC, rate of oxidation of bitumen doubles

2.14.2 Loss of Volatiles

Bitumen consists of some volatile oils that keep it fluid and viscous. When bitumen is
exposed to high temperature for sufficient exposure duration, these oils evaporate and
leave behind a stiff material that has increased viscosity, decreased penetration and
increased softening point. Aging due to loss of volatile oil is more prominent in
viscosity graded bitumen as compared to penetration graded bitumen. In penetration
grade, due to their involatile nature hardening due to loss of volatile is fairly small.

Volatilization of oils can lead to destruction of pavements and resulting in the loss of
ductility of pavements that has damaging effect on functional performance and service
life of the pavement. Exposure conditions such as weather and UV Rays also causes

34
volatilization of asphalt oils that is perhaps considered as important factors regarding
volatilization (Yu, et al., 2012)

2.14.3 Steric Hardening:

Physical hardening or steric hardening of bitumen occurs when bitumen is exposed to

ambient temperatures. The reason behind this hardening is that bitumen molecules
reorientate themselves to adapt to ambient conditions. Steric hardeneing is also caused
by slow crystallization of waxes in bitumen. This is the only type/mechanism of
hardening of bitumen that is reversible. When steric hardened bitumen is reheated, the
original viscosity is regained.

2.15 Types of Bitumen Aging

Aging is normally classified into two broad types:

Short Term Aging

Long term aging

2.15.1 Short term Aging

Shell bitumen Handbook has explained Short term aging as the hardening of bitumen
during mixing with aggregates. During the mixing and production of asphalt concrete,
aggregate and filler is coated with bitumen film of very small thickness usually between
5 to 15 micro meter thick. Thus, favourable conditions for oxidation and loss of volatile
oils occur when bitumen is mixed with aggregates. Aging of bitumen at this point is a
well known phenomenon and is always considered while selecting the grade of bitumen
to be used in asphalt mixture. However, as a rough indication, aging during mixing
process can lead to decrease in penetration by about 30%. Extent of hardening depends
upon several factors at this stage including, bitumen film thickness, mixing temperature
and duration of mixing. To minimize or eliminate the hardness during mixing process,
above mentioned factors must be controlled and among the above mentioned factors,
temperature during mixing is the most critical as mentioned by Bitumen Handbook

35
from shell. Following figure shows increased aging due to increased mixing
temperature as indicated by increased softening point

Figure 2-9 Relationship between softening point and mixing temperature

(Shell Bitumen Handbook)

Following figure shows that as bitumen film thickness is decreased or reduced,

viscosity of bitumen increases as measure by the aging index which is defined as

“ Ratio of the viscosity of the aged bitumen to the viscosity of the virgin bitumen”

Figure 2-10 Effect of bitumen thickness on aging index (Shell bitumen Handbook)

𝑉𝑖𝑠𝑐𝑜𝑠𝑖𝑡𝑦 𝑜𝑓 𝑎𝑔𝑒𝑑 𝑏𝑖𝑡𝑢𝑚𝑒𝑛

Aging index =
𝑣𝑖𝑠𝑐𝑜𝑠𝑖𝑡𝑦 𝑜𝑓 𝑣𝑖𝑟𝑔𝑖𝑛 𝑏𝑖𝑡𝑢𝑚𝑒𝑛

36
 Above figure shows that as film thickness increases, aging index reduces that means
the viscosity of aged bitumen is less than that of the virgin bitumen. (Read & whiteoak,
2003) has mentioned the results of the study of (Haas & S, 1974) in The shell bitumen
handbook concluding that when mixing of asphalt is done in drum it leads to lesser
aged hardening as compared to mixing done in conventional batch mixer. They also
mentioned that drum mixing is efficient perhaps due to less mixing time and presence
of steam in the drum that limits the oxygen thus minimizing the oxidative hardening of
bitumen.

Short term aging can however be controlled to some extent by just using alternative
mixing procedure. Study conducted by Shell bitumen on two different drum mixers
showed that short term aging (increase in softening temperature and reduced
penetration) reduced by almost half of that as when mixing was done using
conventional batch mixing.

2.15.2 Long term aging

As stated earlier that bitumen tends to significantly hardens during mixing and
production of asphalt. Later on, some hardness will also take place during storage and
transportation of bitumen. However hardening does not stop afterwards, infact it
continues to occur even during service life of the pavement. This hardening has been
referred to by “The Shell Bitumen Handbook” as “Long Term Aging”. This behaviour
of bitumen has been shown below

Figure 2-11 Aging of bitumen during mixing, storage and in service (Durability of
bitumen, The shell bitumen handbook)

37
Major factor that contribute to aging during service life of a pavement is the void
content of asphalt mixture. The shell bitumen handbook has mentioned a table that
shows the properties of bituminous mixes after 15 years of service. These mixes have
different void content. Following table shows that when bitumen was recovered from
asphaltic mix with very low void content, its hardening was very less as compared to
bitumen recovered from asphaltic mix of high void content. This is perhaps due to
constant penetration of air and oxygen in asphaltic mix of high void content. Also,
penetration index of mix with high void content was increased appreciably that
indicates the hardening of bitumen and can make asphalt more susceptible to cracking.

Table 4 Properties of Aged samples (The Shell Bitumen Handbook)

According to a research conducted by LUBBERS H E, he studied the bitumen

properties in an asphalt mix that was 5 years old. Results indicated that with void
content of 5% or less, bitumen hardened to very small extent however at void content

38
of 9%, significant hardening took place with penetration value falling from 70mm to
less than 25 mm. (Lubbers, 1985).

It has been observed that bitumen tends to get hard very quickly when in service on
road instead when it is in bulk storage. Following reasons have been identified for this
phenomenon:

• During service life of pavement, there is constant supply of fresh oxygen.

• There can be incidents of fire or extreme temperatures on the road that causes
the loss of volatile oils from bitumen, making it stiff.
• Bitumen can be hardened by oxidation particularly photooxidation caused by
the UV rays from sun.

2.16 Effect of Aging process on properties of bitumen

(Dessouky, et al., 2011) studied the effect of heating duration and temperature
conditioning on the rheological properties of bitumen and performed Bending beam
rheometer, rotational viscometer and dynamic shear rheometer by using both modified
and unmodified binders. These binder were tested at 143oC and 185oC heated at 30
minutes, 2 hours and 4 hours heating duration. Short term aging was also simulated
using rolling thin film oven test. They suggested the heating temperature of 143oC and
duration not to exceed 2 hours.

Figure 2-12 Viscosity at different oven heating duration (Dessouky, et al., 2011)

39
Their temperature limit is contrary to AASHTO (Standard specification of
transportation material and methods of sampling and testing 30 edition) limit that says

“Heating unaged asphalt to temperatures above 135oC should be avoided. however,

with some modified asphalts or heavily aged bitumen, pouring temperatures above
135oC may be required ... do not heat the bitumen above 163oC ... Minimize the
heating temperature and time to avoid hardening the sample”

Viscosity measurements using DSR test showed that 2 hours duration resulted in lowest
increase in viscosity for unaged and RTFO aged bitumen. Bitumen properties such as
complex modulus and viscosity were not affected very much with heating duration.
This was confirmed by DSR sweep test carried out at temperature range of 35oC to
110oC with frequency of 10 rad/sec.

Other researchers such as Suleiman Arafat Yero and Mohammad Rosli Hainin also
studied the effect of STA on bitumen properties. They also simulated STA by RTFO
ASTM D 2872 like (Dessouky, et al., 2011) and determined bitumen properties after
aging. Temperature at which RTFO was performed was 163oC and for duration of 70,
85, 100 minutes for PEN 80/100 bitumen. Results from this study also supported the
literature that aging increases the viscosity while penetration is decreased followed by
elevation in softening point. Since penetration is decreased meaning that bitumen is
more stiff than unaged binder. This stiffness can be related to increased internal
cohesion of bitumen. They also showed that penetration of binder may also depend
upon the source of binder irrespective of time used for aging. Although both binder
showed decrease in penetration as compared to unaged binder but Binder A has shown
slightly less penetration as compared to Binder B (Yero & Hainin, 2012). (Mishra &
Singh, 2019) studied the effect of bitumen aging and roughness of aggregate on
bitumen bond strength and similarly to the above mentioned, they also used RTFO
aging process while they measured the bond strength using Energy Ratio by Surface
free energy results indicated that bond strength increased with increase in aging
temperature and roughness of aggregates.

Aging of bitumen not only affects rheological properties but chemical properties are
also affected as shown by (Yang, et al., 2018) they studied the relationship between

40
micro-structure and mechanical behavior of bitumen by performing DSR and Fourier
transform spectroscopy. Aging enhanced the surface roughness of bitumen. Aging also
resulted in increased carbonyl, sulphoxide and aromatic rings functional group. As far
as rheological properties are concerned, storage modulus increased

41
 CHAPTER 3

EXPERIMENTAL
WORK

42
3.1 Experimental Work

This section covers all the essential details regarding number of samples, samples
conditioning time, temperature at which binder was heated, temperature range and
testing procedures.

As stated earlier, we chose to perform two tests that were rolling bottle test and bitumen
bond strength test. Both of these tests require different sample preparation methods and
will be explained separately.

3.1.1 Temperature range

According to Attock oil Refinery Limited, Mixing temperature for their 60/70 PEN
grade bitumen is 156oC. At this temperature, properties of bitumen are most suitable
for asphalt mix. Our aim was to determine the effect of overheating temperature above
the mixing temperature on adhesion. So for that to achieve, we chose 4oC increments
above mixing temperature i.e 156oC and continued to perform test by increasing
temperature until significant stripping was observed

When we tested sample at 172oC, much stripping was observed in rolling bottle test
and bitumen bond strength for 172oC indicated value below 2 MPa so we stopped the
test. Thus, our temperature range was.

156oC 160oC 164oC 168oC 172oC

3.1.2 Number of Samples

Two samples at each temperature were tested both in case of rolling bottle test and
bitumen bond strength test then their results were averaged. So, 10 samples were
prepared for rolling bottle test and for bitumen bond strength test also giving a
cumulative number of samples that were tested as 20.

43
3.1.3 Sample preparation for Bitumen Bond Strength test

Bitumen Bond Strength test was performed in accordance with AASHTO T 361. It
requires aggregate substrate, metal ring, pneumatic adhesion tensile testing equipment,
reaction plates , pullout stubs and oven. Binder was heated at 156oC, 160oC, 164oC,
168oC, 172oC for 50 minutes in an oven until binder was fluid enough for proper mixing
since (dessouky, et al., 2011) suggest to use less than 2 hours heating. Binders were
then applied on stubs and allow it to cool for 10 to 20 seconds then pressed firmly on
aggregate substrates. Stubs must be pressed as straight as possible to avoid entrapped
air bubbles. Apply downward force until stub reaches the plate. Excess binder will flow
out through the channels provided in pullout stubs.

Before application of binder on pullout stubs, stubs were heated in an oven to remove
any moisture at temperature of 150oC for 20 minutes. 5 aggregate substrate plates were
used with dimensions of 6” x 6” x 1”. These plates were washed to remove any dust
particles and contaminants and then placed in an oven for about 1 hour to let them dry
completely.

After the application of binder on stubs and then pressing stubs on aggregate plates or
substrate. They are allowed to stay at room temperature for 24 hours prior to testing.
We only performed dry test since only effect of overheating on adhesion of bitumen
was to be assessed and not the moisture damage. Of course, wet test gives less values
as compared to dry test due to presence of moisture in addition to other parameters.

3.1.4 Sample Preparation for Rolling bottle test

Binders were heated at same temperatures and for same duration as for BBS test.
Rolling bottle test was performed in accordance with BS EN 12697-11:2005. It requires
loose asphalt mix. European standard has three types of aggregate fractions to be used
in RBT 5/8mm, 6/10mm, 8/11mm.. we chose 6/10 mm that means passing of 10 mm
sieve and retained of 6 mm sieve because according to Standard if 5/8 mm fraction is
used that may result in formation of lumps and visual observation is affected. Prior to
mixing aggregates were washed to remove any dust particles and contaminants that

44
may interfere with the mixing process. they were then placed in oven for 1-2 hour at
110oC. About 170 g of sieved aggregates were taken and then about 7 to 8 grams of
heated binder at each above mentioned temperature was added that corresponds to
approximately 4% binder content. Aggregates and binders were mixed thoroughly to
coat all aggregates uniformly. Prepared samples were then placed on silicon sheets at
room temperature for conditioning. Also rolling bottles were washed thoroughly prior
to addition of aggregates

Figure 3-1 Rolling bottle test sample for 24 hours conditioning at room temperature

3.1.5 Bitumen Bond strength test procedure

After the preparation of sample and proper conditioning. Adhesion testing equipment
consists of Gasket, Piston, rate control, Air hose, Run button, metal ring support and
Reaction plate.

Calibrate the instrument by apply air pressure for 3 seconds. After that loading rate was
set to 100psi/sec as specified by AASHTO T 361. Next ring support and metal ring
supports were placed around the stubs. Then gasket was screwed with pullout stub and
piston was placed on it. After final placement of reaction plate on the piston, device
was started and pressure was applied until stubs were detached from aggregate

45
substrate. Bursting pressure from device was noted and Pull Off Tensile Strength was
determined from formula as given Below.

(𝑩𝑷 𝒙 𝑨𝒈) − 𝑪
𝑷𝑶𝑻𝑺 =
𝑨𝒑𝒔

POTS = Pull off tensile strength (MPa)

BP = Bursting pressure (MPa)

Ag = Contact area of gasket (mm2) = 2619.3 mm2

C = Piston Constant = 129.73

Aps = 126.64 mm2

Figure 3-2 Components of BBS Test

3.1.6 Rolling bottle test procedure

After sample preparation and 24 hours conditioning, sample was placed into rolling
bottles made of Borosilicate material. Sample was detached from each other and one
particle at a time was put into bottle. Glass stirrer was then placed and filled with
distilled water upto the mark. Rotation speed was set to 60 rotations/minute because

46
BS EN 12697-11:2005 suggest to use 60 rotations/minutes for binder with penetration
less than 100 mm. bottles were then placed on rolling machine and started to roll. After
6 hours rolling process was stopped and aggregates were taken out and bitumen
coverage was visually observed then same procedure was repeated after 24, 48 and 72
hours of rolling time. There exists a great variation in the results because of the visual
observations therefore, observation by two observers were taken and then averaged.

Figure 3-3 rolling bottle test assembly

3.1.7 Flow Chart

Following flow chart summarizes our Experimental program.

47
 Experimental
Work

No. of Heating Sample

samples temperatures Preparation

24 hours of
Rolling bottle Bitumen Bond 156oC, 160oC, Sample
test Strength test 164oC, 168oC, Conditioning
172oC

2 samples at 2 samples at
Sample
each each
Testing
temperature temperature

Rolling bottle Bitumen Bond

test Strength Test

Visual Observation Bursting pressure

after 6, 24,48 and 72 from device
hours of rolling time

Figure 3-4 Experimental work Flow Chart

48
 CHAPTER 4

RESULTS AND
DISCUSSIONS

49
4.1 Results

Two tests were performed to study the effect of overheating on adhesion of asphalt
binder. The results are discussed as below.

4.1.1 Bitumen Bond Strength Test

Bitumen Bond strength Test was performed on overheated bitumen samples with two
samples at each temperature increment. BBS test was performed in accordance with
AASHTO T 361 and samples were conditioned for 24 hours at room temperature.
Bursting pressure was noted from PATTI equipment in PSI and then this pressure was
converted to MPa and then Pull off tensile strength was determined using area of
reaction plates, and area of pull off stub Shown in Table 4.

Table 5 Bitumen Bond strength Test results

Bitumen bond Strength Test

Ag 2619.3 mm2
C 129.73
Aps 126.64 mm2
Bursting Average
Temperature Bursting Pull-off tensile
pressure bursting
(°C) pressure (Mpa) strength (MPa)
(Psi) pressure
29
156 28.5 0.196 3.04
28
28.1
160 26.55 0.183 2.76
25
27
164 25.1 0.173 2.55
23.2
22
168 21.75 0.15 2.07
21.5
21.5
172 18.6 0.128 1.62
15.7

50
Two bursting pressure at each temperature increment was obtained that was then
averaged to get average bursting pressure for that temperature.

Pull off tensile strength indicate that that as bitumen is heated above its mixing
temperature i.e., when heated above 156oC, amount of energy required to detach the
pull off stub from aggregate plate decreases that indicates the loss of adhesion between
bitumen and aggregate. When results were plotted against Temperature on X axis and
pull off tensile strength (POTS) on Y axis, a downward trend was observed as indicated
by Figure 17 Graph below.

Bitumen Bond Strength Test

3.5
PULL OFF TENSILE STRENGTH

3.04
3 2.76
2.55
2.5
(MPA)

2.07
2
1.62
1.5

1
156 160 164 168 172
MIXING TEMPERATURE OC

Figure 4-1 Graph between Temperature and Pull off Tensile Strength

POTS decreased from 3 MPa at 156 °C to 1.6 MPa at 172 °C. Considering the initial
increment of 4 °C, loss in POTS is small as indicated by POTS value at 156 °C and
160°C as 3.04 MPa and 2.76 MPa Respectively. As temperature was further increased
loss in POTS increased. After 8oC increment above the mixing temperature POTS
dropped further up to 2.55 MPa. Loss in POTS can be attributed to the fact that many
researchers (Nurfazilah, 2012) (Mishra & Singh, 2019) (sarnowski, et al., 2019)
(baidya & singh, 2019) have concluded that when bitumen is overheated at high
temperatures then after certain temperature loss of volatile oils take place and aging
starts. Vaporization of oils leaves behind stiff material that is not absorbed properly

51
into the pores of aggregates and proper mechanical interlocking does not occur leading
to poor adhesion and less amount of energy required to detach the stub.

4.1.2 Rolling bottle test

Rolling bottle test was performed at 156oC, 160oC, 164oC, 168oC, 172oC and visual
observations were taken after 6, 24, 48 and 72 hours. Photos of samples are presented
in Annexure-B

Each image was carefully analysed by two separate observers and their observations
were averaged. Graphs shown below indicate that as bitumen is overheated above its
mixing temperature, stripping increases and resistance against durability decreases.

Rolling Bottle Test

Bitumen Coverage After 6 Hours
100 90
85 80
90
75
80
Percentage Coverage

65
70
60
50
40
30
20
10
0
152 156 160 164 168 172 176
Mixing Temperature oC

Figure 4-2 Bitumen Coverage after 6 hours of rolling time

After 6 hours of rolling time, the results indicate that bitumen heated at 156oC shows
most durability against moisture damage with only 10 % loss in bitumen coverage and
loss of coverage increased as the temperature was increased with 35 % loss in 172o C
sample. When heated at 4oC increment above 156oC, bitumen coverage dropped from
90% at 156oC to 85% at 160oC, this indicates that bitumen was further stripped up to
15% by an increment of 4oC. Similarly, after 8oC increment from mixing temperature,
bitumen coverage of 80% was observed during first 6 hours of rolling time. Bitumen
coverage of 65% was observed when heated at 172oC as compared to virgin bitumen
at 1560oC that showed coverage of 90% after 6 hours rolling time.

52
 Rolling Bottle Test
Bitumen Coverage After 24 Hours
100
75

Percentage Coverage
80 70
60
55
60 45
40

20

0
152 156 160 164 168 172 176
Mixing Temperature oC

Figure 4-3 Bitumen Coverage after 24 hours of rolling time

Also, after 24 hours of rolling time, the bitumen coverage loss in 156oC sample was 25
% as compared to the loss of 10% at 6 hours rolling time and 172oC sample showed
poor durability exhibiting 60% loss in coverage even after 24 hours of rolling time.
Comparison between these two temperatures exhibited the loss of 46 %. At 160oC,
bitumen coverage decreased from 85% to 70% after 24 hours of rolling time. The
trendline indicates that as we increase the mixing temperature, the resistance against
moisture damage decreases with increased stripping.

Rolling Bottle Test

Bitumen Coverage After 48 Hours
100
Percentage Coverage

80
60
60 45 40 35
40 25
20
0
152 156 160 164 168 172 176
Mixing Temperature oC

Figure 4-4 Bitumen Coverage after 48 hours of rolling time

Similarly, after 48 and 72 hours, same trendline is observed with increasing percentage
loss in stripping. The decreased bitumen coverage with increase in temperature can be

53
attributed to the short term aging that may have occurred during heating and mixing
and caused bitumen to become stiff.

Rolling Bottle Test

Bitumen Coverage After 72 Hours
100
90
80
Percentage Coverage

70
60
50 40 40
35
40
25
30
15
20
10
0
152 156 160 164 168 172 176
Mixing Temperature oC

Figure 4-5 Bitumen Coverage after 72 hours of rolling time

Results indicate that after 164oC durability against moisture damage decreases
drastically that is indicated by bitumen coverage of 25% at 168oC after 72 hours of
rolling time. When heated at 168oC and 172oC bitumen coverage is much less i.e 25%
and 15% respectively, that is the indication of poor adhesion between bitumen and
aggregates. This is because after 164oC, loss of volatile oils started to occur and aging
process started that effects the wettability of aggregates by bitumen due to its increased
stiffness and increased viscosity thus bitumen is not properly absorbed into the pores
of aggregates to create a strong bond.

4.1.3 Comparison of loss in adhesion in both tests:

By taking the maximum value of pull of tensile strength and bitumen coverage after 72
hours as reference point with zero percent loss and comparing it with values obtained
at overheated temperatures, following bar chart is obtained.

54
 Table 6 Percentage Loss in adhesion

Rolling Percentage
Percentage
Mixing Bottle loss in
loss in
Temperature BBS after adhesion
adhesion
( °C) 72 (Rolling
(BBS)
hours bottle)

156 3.04 42.5 0 0

160 2.76 38.75 9.21 11.1

164 2.55 35 16.1 22.2

168 2.07 28.75 31.6 33.3

172 1.62 17.5 46.3 55.5

BBS and Rolling Bottle Test

Comparison
60 55.5
Percentage loss in adhesion

50 46.3

40
31.6 33.3
30
22.22
20 16.1
11.11
9.21
10
0 0
0
156 160 164 168 172
Mixing temperature oC

BBS Rolling Bottle Test

Figure 4-6 Percentage Loss in adhesion

55
The graph shows approximately similar losses in adhesion between two tests performed
except one significant difference at 172oC. This confirms that adhesion of bitumen with
aggregates decreases when bitumen is heated over its mixing temperature. The
percentage loss on average between 4oC is shown in table and graph below.

Table 7 Percentage Loss per 4° Celsius

Percentage loss in Percentage loss in adhesion Average Loss per

adhesion (BBS) (Rolling bottle) Loss 4 °C
0 0 0 0

9.21 11.1 10.155 10.16

16.1 22.2 19.15 9.00

31.6 33.3 32.45 13.30

46.3 55.5 50.9 18.45

Percentage Loss per 4°Celsius

20 18.45
18
16
13.3
14
Percentage Loss

12 10.16
10 9.00
8
6
4
2 0
0
156 160 164 168 172
Mixing temperature oC

Figure 4-7 percentage Loss per 4° Celsius

56
This indicates that on average percentage loss between 156oC to 164oC is 9.5 % on
average while after 164oC, it increases exponentially. Thus, 164oC temperature can be
taken as maximum point after which if bitumen is heated, shall not be used in road
construction purposes as adhesion is decreased exponentially.

57
 CHAPTER 5

IMPACT OF THIS
RESEARCH

58
5.1 Case Study

Its has been established till yet that overheated bitumen during asphalt mixing can cause
early stiffness of binder and can make asphalt to behave as brittle material. This
stiffness of binder can have significant impact on economy, service life of pavement
and natural resources which is discussed below

Consider the following scenario, two flexible pavements with Structural Number SN 3
have been constructed. Let’s say, the length of both pavements is 10 Km. Assuming
the initial cost for both pavements to be 100 million rupees. This cost includes material
cost, machinery and labour cost and all finishing works cost. Both pavements were
designed for the service life of 10 years. Let’s just take average maintenance cost of
pavement as 3 million rupees per Km. Assuming that the normal pavement require
rehabilitation after 5 years.

Asphalt was prepared in asphalt plant. Let’s name the Pavements as Pavement 1 and
Pavement 2. For these pavements, asphalt from two different plants were used. For
pavement 1, asphalt was prepared in full controlled environment including controlled
material usage with proper design specifications and desired material proportions. For
this asphalt mix, bitumen was heated at prescribed mixing temperature under strict
quality and temperature control. Process of short term aging was avoided due to proper
temperature control. It was then mixed with aggregates and filler to form a uniform
asphalt mix which was transported to the site. It was then laid and compacted with the
help of rollers.

For Pavement 2, asphalt mix from 2nd plant was used where bitumen was heated at
temperature without any control and any strict observations, in this way binder got
overheated and the process of short term aging started during mixing. Asphalt mix got
stiff and became brittle as compared to the pavement 1 which would have flexible
behavior since bitumen was heated in controlled environment

59
5.1.1 Cost effectiveness
As it is an established fact that when asphalt is in service, long term aging takes places
due to oxidation, UV rays, Loss of volatiles etc. Now pavement 1 has not experienced
short term aging, it will have long term aging that is a slow process. While pavement 2
has already experienced short term aging due to over heating of binder. This short term
aging affected the bitumen coverage and adhesion of bitumen with aggregates. When
in service, long term aging also started and as pavement 2 was already aged so further
worst scenario develops leading to formation of cracks under vehicular load and due to
moisture damage. This pavement failed in its early years prior to the completion of its
design life. the pavement was designed for the design life of of 10 years and if it
requires asphalt overlay after every 2 years, its maintenance cost will be 150 million
rupees over its full design life that will be much higher as compared to pavement 1 that
was formed using asphalt mix with proper temperature control and after 2 years
pavement 1 required very little or no rehabilitation. In this way, just by controlling the
heating temperature of bitumen while mixing, rehabilitation cost of pavements can be
reduced to much degree.

5.1.2 Resource Utilization

Also, when asphalt overlay was applied it required aggregates and bitumen. In this way,
natural resources will also be used in great quantity during rehabilitation after every 2
years in case of pavement 2 as compared to pavement 1. Thus, natural resources such
as aggregates and bitumen can also be saved simply by controlling the mixing
temperature of bitumen.

5.1.3 Ride quality

Pavement 1 will provide smooth ride quality as compared to pavement 2. Since
stripping will occur and crack would appear in pavement 2 due to brittle nature and use
of aged bitumen in asphalt mix that will cause bumpy surface. Thus, ride quality can
also be improved and maintained for longer duration during the design of life pavement
just by controlling the temperature during production of Asphalt mix.

60
 CHAPTER 6

CONCLUSIONS AND
RECOMMENDATIONS

61
6.1 Conclusions

According to the results obtained and after analyzing them, following conclusions are
drawn:

• As the mixing temperature is increased beyond the prescribed mixing

temperature 156 °C, the pull off tensile strength is decreased. The decrease is
9.21 % loss in strength at 160 °C, 16.1 % at 164 °C, 31.6 % at 168 °C and 46.3
% at 172 °C when compared with strength at 156 °C.
• Similarly, durability against moisture damage is decreased. The percentage loss
in durability against moisture damage at 160 °C is 11.1 %, at 164 °C is 22.2%,
at 168 °C is 33.3 % and at 172 °C is 55.5 % when compared to durability against
moisture damage at 156 °C.
• This decrease in adhesion properties is due to loss in volatile oils, aging of
bitumen and increased viscosity of bitumen after overheating. This is in
accordance with the results of many researchers that also studied the
overheating phenomenon of bitumen (Nurfazilah, 2012)
• As the loss between 156-164 °C is less and after 164 °C the loss is doubled, the
maximum mixing temperature of 60/70 grade of Attock Oil Refinery should not
increase from 164 °C for best performance of roads.
• Overheating after 164 °C because of negligence and improper equipment can
cause huge losses in performance due to stripping and pavement fails before the
completion of design life.
• Moreover, the percentage loss depicted by both rolling bottle and Bitumen bond
strength test is approximately equal. So only one of these tests is enough to
assess the adhesion of bitumen with aggregate

62
6.2 Recommendations

Recommendations are made as follows:

5.2.1 For Road Construction purposes:

Following are the recommendations for road construction purposes:

• Proper instrument shall be used for controlled heating.

• Skilled labor shall be employed for this work.
• If bitumen gets overheated after 164 °C, it should be discarded.

5.2.2 For Future Work:

Following are the recommendations for future work in this area:

• Performance of all other grades shall be checked against overheating and

comparison shall be made with these values.
• Performance of bitumen from other sources shall be checked against
overheating.
• Performance of aggregates from different source shall be checked.
• Following tests shall be performed which are not included in this study
including Static water storage test, Contact angle measurement test and boiling
water test.
• As similar results in terms of percentage loss is obtained between BBS and
Rolling Bottle Test, only one test can fulfill the purpose.

63
WORK CITED

64
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ANNEXURE A
BITUMEN BOND STRENGTH TEST

70
 Figure A-1 Failure surface at 156oC

Figure A-2 Failure surface at 156oC

Figure A-3 Failure surface at 160oC

Figure A-4 Failure surface at 160oC

Figure A-5 Failure surface at 164oC

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Figure A-6 Failure surface at 168oC

Figure A-7 Failure surface at 168oC

Figure A-8 Failure surface at 172oC

Figure A-9 Failure surface at 172oC

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ANNEXURE B
ROLLING BOTTLE TEST

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 156oC
Sample A Sample B
6 hours rolling time

24 hours rolling time

74
48 hours rolling time

72 hours rolling time

75
 160oC
Sample A Sample B
6 hours of rolling time

24 hours of rolling time

76
48 hours of rolling time

72 hours of rolling time

77
 164oC
Sample A Sample B
6 hours rolling time

24 hours rolling time

78
48 hours rolling time

72 hours rolling time

79
 168oC
Sample A Sample B
6 hours rolling time

24 hours rolling time

80
48 hours rolling time

72 hours rolling time

81
 172oC
Sample A Sample B
6 hours rolling time

24 hours rolling time

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48 hours rolling time

72 hours rolling time

83