Construction and Building Materials 308 (2021) 125135

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Construction and Building Materials

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Moisture susceptibility and fatigue performance of asphalt binder modified

by bone glue and coal fly ash
Junaid Muhammad a, Tianyi Peng a, Weiguang Zhang a, *, Hanglin Cheng a, Haroon Waqas c,
Samad Abdul a, Kunwei Chen a, Yang Zhou b
a
School of Transportation Engineering, Southeast University, Nanjing, Jiangsu, China
b
School of Materials Science and Engineering, Southeast University, Nanjing, Jiangsu, China
c
Department of Civil Engineering, Faculty of Engineering and Technology, International Islamic University, Islamabad, Pakistan

A R T I C L E I N F O A B S T R A C T

Keywords: The main purpose of incorporating waste into asphalt binder is due to their excellent properties and low cost as
Bone glue (BG) binder modifiers, in contrast to the impracticability of typical binder in the current flexible asphalt pavement by
Coal fly ash (CFA) the increase of heavy traffic loads and volumes. The focus of this study is to use coal fly ash (CFA) with bone glue
Modified asphalt
modified asphalt to check the effect of coal fly ash (CFA) towards fatigue resistance and moisture sensitivity. This
Fatigue resistance
study combined 60/70 penetration grade binder with optimum percentage of bone glue (10%) and 2%, 4%, 6%
Moisture sensitivity
and 8% of fly ash. After conducting consistency tests and some mixture tests, it is concluded that fly ash gives
superior fatigue life to flexible asphalt pavement and the effect towards moisture sensitivity is slightly good.

1. Introduction asphalt binder from PG-58 to PG-70. It can also reduce permanent
deformation to a range between 28% and 42% based on laboratory
Due to increasing number of populations, traffic volumes increased testing at temperatures of 40 ◦ C and 55 ◦ C. The decrease in rut depth
traffic loads, which effect the pavement service life, more and more may attribute to higher stiffness of bone glue-modified asphalt. One
materials with high durability are required during road construction and problem of applying BG, as reported elsewhere, is the moisture damage
maintenance process [1-3]. It leads to the demand of binder modifiers/ potential if the asphalt mixture was not well mixed [11].
additives to modify the neat asphalt binder to meet the specific re­ When increasing the rutting resistance of asphalt binder, it was un­
quirements of pavement structure, such as rut resistance, low temper­ known that if the BG can affect the fatigue resistance of asphalt binder.
ature resistance, and fatigue resistance [4-6]. The use of modifiers seems The fatigue life is an important factor of flexible asphalt pavement and
to be the best appropriate option to overcome this situation, as it is mostly the fatigue distress in pavements occur due to low temperature
known that the modified binder has the capability to boost the perfor­ [12-14]. There are many ways to improve the fatigue life and reduce
mance of pavement structure because they exhibit improved rheological moisture sensitivity by using different types of chemical additives,
properties [7-10]. modifiers, fillers etc. [15,16]. One of the most efficient materials is
Bone glue (BG) is a widely seen waste in Pakistan. It is a protein- called coal fly ash (CFA) which is a by-product of coal combustion
based gum prepared from collagen which is generated from animal process and is generated during electricity production in thermal power
skeletons and their meat excrete. The collagen is a network of proteins plants [2]. The annual generation of CFA is one billion tones globally
and its major part can be obtained from animal bones which takes and it’s dumping causing many environmental problems. CFA exhibits
approximate 20% to 35% protein of the whole body. The BG is yel­ pozzolanic activity due to which it is used in variety of application such
low–brown in color and is soluble to asphalt binder and hot water. The as in road construction (mainly embankments [17], subgrade stabili­
typical pH value of BG is between 5.8 and 6.3 which makes it good to zation [18], base layers [19] etc.), problematic soil improvement [20],
stick to aggregate. The measured density of BG is approximately 16.57 and concrete [21].
with viscosity of 83.3 cp at room temperature. The potential of applying Therefore, the research objectives of this research work are as
BG to modify asphalt binder attracts more and more attention. It was follows:
found that the addition of BG result in bumped high temperature PG of

* Corresponding author.

https://doi.org/10.1016/j.conbuildmat.2021.125135
Received 11 June 2021; Received in revised form 29 September 2021; Accepted 30 September 2021
0950-0618/© 2021 Elsevier Ltd. All rights reserved.
J. Muhammad et al. Construction and Building Materials 308 (2021) 125135

Fig. 1. Experimental program flow chart.

Table 1 Table 2
Basic properties of the binder. Physical properties of aggregates.
Test Values Standard Used Test / Property Test Results (%) Max/Min Limit

Softening point (◦ c) 47 ASTM D36 Los Angeles abrasion 14 15% (max)

Penetration (0.1 mm, at 25 ◦ c) 69.5 ASTM D1586 Water absorption 1.01 2%(max)
Ductility (cm) 97 ASTM D113 Elongation 12.5 15% (max)
Flash point (◦ c) 235 ASTM D92 Flakiness 14 15% (max)
Fire point (◦ c) 240.5 ASTM D92 Crushing Value 23 40% (max)
Specific gravity 0.96 ASTM D1298 Impact Value 12 10–20%

To determine the effect of CFA as a modifier in order to enhance the remove fuels and lubricants. The basic properties of asphalt binder are
fatigue resistance of bone glue asphalt. presented in Table 1.
To investigate the adhesion potential of CFA modified BG asphalt The coarse and fine aggregates were obtained from Margallo hills
binder and its impact on moisture susceptibility of modified BG located near Islamabad. The basic properties of Margallo aggregates are
asphalt mixtures. presented in Table 2. The qualitative tests of aggregates were checked as
To investigate the fatigue behavior of CFA modified BG asphalt per AASHTO and ASTM standards. Rounded and river bed gravels were
mixture. avoided in this experimental work. NHA class B gradation was used in
this study and presented in Fig. 2.
2. Materials and methods CFA is a fine powder that is a by-product of burning pulverized coal
in electric generation power plants. CFA is a pozzolan, a substance
This study selected CFA as an additive for making blend with BG- containing aluminous and siliceous material that forms cement in the
modified asphalt. The testing program (Fig. 1) included the CFA and presence of water. When mixed with lime and water, CFA forms a
BG-modified binder and conventional binder characterization through compound similar to Portland cement. CFA ash was obtained from local
penetration, softening point, ductility and flash and fire point tests. The available supplier. Bone glue is a strong, liquid, protein-based adhesive
storage stability test was incorporated to study the dispersion of each made from collagen in bones, sinew, and cartilage. Bone glues are
CFA and BG-modified binder. Chemical characterization was carried out considered inferior to skin and parchment glues. They are often sold in
using Fourier Transform Infrared Spectroscopy (FT-IR) [22]. Then the granular form instead of sheets. Bone glues are used as carton and box
CFA and BG-modified binder was combined with the aggregates for the adhesives. Bone glue was obtained from local available market.
preparation of asphalt mixtures, which were tested for stiffness (dy­
namic modulus) [23], fatigue cracking (four-point-bending-beam-fa­ 2.2. BG-modified asphalt preparation
tigue) [24] and moisture induced damage which was calculated using
rolling bottle test (RBT) and bitumen bond strength test (BBS) [25]. In this study, Rizvi et al mixing technique was adopted for successful
dispersing the BG into the asphalt binder [26]. Before mixing BG with
2.1. Materials binder, first dissolve into the appropriate amount of water for satisfying
proper mixing. Specific mixing time and temperature were followed
The penetration grade 60/70 has been used in this research work. shown in Table 3.
The binder has extensively been used on highways and motorways Hand mixing was avoided in this paper as Asif et al. [27] recom­
which are carrying approximately 75% of the total road freight. The mended that it doesn’t ensure complete mixing of BG in bitumen. So, a
asphalt binder is a co-product of the petroleum-refining system that shear homogenizer was used for ensuring proper mixing of BG in
produces gasoline, diesel fuel, lubricating oil, as well as several other bitumen.
petroleum products. The asphalt binder is produced from the thick, The results of proper mixing were checked with the help of FTIR
heavy residue (residuum) that remains after distillation of petroleum to (Fourier transform infrared spectroscopy). The FTIR results for neat and

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J. Muhammad et al. Construction and Building Materials 308 (2021) 125135

Fig. 2. Mid-point gradation curve of aggregates.

for blows on the mixture having weight of 4.5 lbs. which has a height of
Table 3 fall of 18 in. and no. of blows used were 75 for each sample. Marshall
Mixing time and temperature for preparation of modified binders.
Mix design was performed only for neat binder and the optimum binder
BG and FA modified Mixing Mixing Physical appearance content result of neat binder were kept same for all other samples to
blend temperature (◦ C) Time (min.) allow comparability and consistency of test results [28,29].
10% BG by weight of 130 55 Settled FA particles One other reason is to check the optimum binder content variation
binder and free of bubbles effect on different rheological and mixture properties of the binder.
2% FA in BG-modified 115–130 20
From the literature it is observed that change in optimum binder content
binder by its weight
4% FA in BG-modified 26 for neat and BG- modified binder is very less i.e. 0.06–0.25% which is
binder by its weight very less in terms of weight. So, for the ease of researchers and to check
6% FA in BG-modified 32 its effects, the OBC used in this study is same for neat and modified
binder by its weight binders.
8% FA in BG-modified 40
binder by its weight
2.5. Experimental program

modified binder were shown in in Fig. 3. Fourier transformed infrared 2.5.1. Consistency test
spectroscopy results of CFA and BG-modified binder show carbon- Consistency tests were performed with three replicates to evaluate
hydrogen stretching and bending frequency properties of a typical hy­ the basic properties of the binder. In this study the effect of BG and CFA
drocarbon FTIR peaks at approximately 1050–1100 cm− 1, 300–500 were checked by performing Penetration, Ductility, Softening Point and
cm− 1, and 10–50 cm− 1 can probably be attributed to the C–H symmet­ Flash and fire point tests as per ASTM D1586 [30], ASTM D113 [31],
ric/asymmetric stretch, C–H bending variation and C–H shocking vi­ ASTM D36 [32] and ASTM D1310 [33], respectively.
brations respectively [26]. FTIR spectrum of the bone glue-modified
asphalt binders is quite similar to that of the neat binder which is an 2.5.2. Storage stability
indication of a homogeneous product. The storage stability of the BG and CFA modified binder were check
by repeating the storage stability test three times per ASTM D5892 [34].
2.3. BG-modified asphalt and CFA mixture preparation In this test the storage stability property were estimated in terms of
separation index (SI). Separation index is the softening point value dif­
After preparation of blend of BG and binder, different percentages of ference of the top and bottom portion of the sample. The sample is
CFA (as suggested by researchers) in this blend were also mixed. For considered as storage stable if the value of SI is less than 2.2 ◦ C as per BS
mixing of CFA in BG and binder we don’t use shear homogenizer. In this EN 13399:2017 [35].
study it is observed that, if we used shear homogenizer for making blend
of CFA and BG-modified asphalt the bubbles arise in the mixture when a 2.5.3. Rolling bottle test
specific temperature achieved, so for ensuring homogeneous mix The purpose of this test is to check the moisture susceptibility of neat
continuous stirring with a stick is necessary. The temperature range for and modified binder. The test was performed according to BS EN
mixing is 120–135 ◦ C. The time for different percentages of mixing is 12697–11 [36]. The results of this test will be measured by visual in­
shown in Table 3. spection in term of the degree of bitumen coating on loose bitumen
coated aggregates after the influence of mechanical stirring in water.
2.4. Asphalt mixture samples preparation The weight of aggregates sample used in this test is 170 gm. (Passing
through 9.76 mm and retained on 6.3 mm sieve) and 8 gm. of asphalt
NHA class B gradation was used for asphalt mixture samples prep­ binder which is approximately 4.5% of the aggregates. Oven dried and
aration. Marshall Mix design (ASTM D 1559) was used, to find optimum clean aggregates particles will coat with a bitumen layer of approxi­
percentage of binder content to be mixed in the mixture. Hammer used mately 0.1 mm thick. Then store these coated aggregates for 12–64 h at

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J. Muhammad et al. Construction and Building Materials 308 (2021) 125135

Fig. 3. FTIR results of neat and modified binders.

room temperature. Before starting the test, filled glass bottles with 2.5.4. Bitumen bond strength test
deionized water and coated aggregates, the height of water is up to the The instrument used for this test is PATTI (Pneumatic Adhesion
shoulder of the bottle. Then add a glass stirrer to the bottles. The bottles Tensile Testing Instrument). BBS test is used to check the adhesion of
were placed in the rolling bottle machine which rotating at 60 rpm, and bitumen with aggregates after 24 h dry and 24 h moisture conditioning
coating of samples were checked after 6, 24, 48 and 72 h. in terms of bond strength of bitumen-aggregate. The standard followed
while performing this test is ASTM D 4541 [37]. A limestone aggregate
plate (15′′ × 6′′ × 1.5′′ ) was used in this test. For sample preparation both

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J. Muhammad et al. Construction and Building Materials 308 (2021) 125135

Fig. 4. Penetration values. Fig. 5. Softening point values.

the limestone plate and asphalt binder were heated at 150 ◦ C to ensure
Table 4
proper adhesion of stubs with aggregates.
Penetration index of BG and CFA-modified bitumen.
For each dry and moisture condition, three samples were tested. The
moisture condition was performed by placing the sample in a water tub Sample PI A
for 24 h at 25 ◦ C. The results of the test was recorded, which is actually Neat Binder − 1.2919 0.0489
the burst pressure at the point of stub detachment. The BBS value is 10% BG + 2% FA − 0.8856 0.0458
recorded in terms of Pull off tensile strength (POTS) by using the below 10% BG + 4% FA − 0.7676 0.0449
10% BG + 6% FA 0.7478 0.0358
equation. 10% BG + 8% FA 0.8015 0.0355
(BPxAg) − C
POTS = (1)
Aps
3. Results and discussions
where Ag is the contact area of the gasket with reaction plate, Aps is the
3.1. Penetration index
pull-out stub area, C is piston constant and BP is burst pressure.
The value of Ag is 4.06 in2, C is 0.286 in2 and for Aps is 0.193 in2.
The BG and CFA modified asphalt binder sensitivity to temperature
These values are for specific stub type which is F-4, used in this study.
were checked with the help of its penetration index (PI). The term PI is
dependent on penetration and softening point values of the asphalt
2.5.5. Dynamic modulus test
binder. The penetration test measures the stiffness of the selected binder
This test is used to check the permanent deformation resistance of
at room temperature. In other words penetration index represents the
the asphalt mixture. The cylinder-shaped sample was prepared with the
quantitative measure of the reaction of asphalt binder to variation in
help of super pave gyratory compactor (150 mm diameter and 170 mm
temperature. If the penetration value decreases from higher to low, it
height of sample). Mixing temperature is 160 ◦ C and 600 kPa pressure
means the binder become stiffer and resistance to loading increases
were applied to achieve the desire height. A sample extracted from
[40]. The decrease in penetration values were noted in term of per­
compacted sample having 150 mm height and 100.5 mm diameter for
centages which is 3.13%, 18.22%, 18.02% and 35.28% for 10% BG
dynamic modulus testing. After preparation of samples, the dynamic
content and 2%, 4%, 6%, and 8% of CFA respectively as shown in
modulus of asphalt mixture was determined by Cooper NU-14 test ac­
(Fig. 4). Softening point results shows that at which temperature the
cording to AASHTO TP 62-03 [38]. Loading of 525 kPa and 195 kPa in
bitumen will deform [41]. In this study the softening point of the
the form of sinusoid with varying load frequencies (25, 10, 5, 1, 0.5, and
modified bitumen was increased from 46 at 75 ◦ C to 58 at 125 ◦ C. The
0.1 Hz) was applied at 21 ◦ C and 38 ◦ C correspondingly with three
values are presented in (Fig. 5).
replicate samples.
The PI can calculate with the help of the following equation.
2.5.6. Four-point bending beam fatigue test 20 − 500A
PI = (2)
The fatigue resistance of asphalt mixture was assessed by four-point 1 + 50A
bending beam fatigue test following AASHTO T321 standard [39]. For
performing this test, a roller compacted slab of size 380 mm × 250 mm Where,
× 63 mm with target air voids of 5.5% were prepared. Then a beam [log(800) − log(PenatT) ]
samples were trimmed from each slab of size 380 × 50 × 63 mm. Test A= (3)
SP − 25
was conducted in strain-controlled approach on HMA beam samples in
repetitive four-point loading at 300 micro strain (με). The testing tem­ In the above equation T is the penetration test temperature, which is
perature was 20 ◦ C and frequency was 10 Hz with three replicate sam­ 25 ◦ C, Pen at T shows the penetration test value at desired temperature T
ples. The output of this test is no of loading cycles to failure, which is (0.1 mm), SP represent the softening point of the asphalt binder (◦ C),
considered as fatigue life of asphalt mixture. and Pen at SP means penetration at the softening point and assumed as
800 (0.1 mm) [42].
Most of the asphalt binder have PI values in the range of − 2 and + 2,
which means that an asphalt binder having higher PI value will be less
susceptible to temperature and vice versa [43]. The results of PI index
and thermal susceptibility (A) is presented in Table 4 (Fig. 6)

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J. Muhammad et al. Construction and Building Materials 308 (2021) 125135

Fig. 6. Effect of CFA and BG on penetration index (PI) and thermal susceptibility (A).

Fig. 7. Effect of CFA and BG on ductility values. Fig. 9. Separation index values graphical representation.

binder decreases the ductility values, which means that the stiffness of
the binder increases [44], presented in (Fig. 7). The flash and fire point
results tell us about the safe mixing and application temperature. At
higher temperature the bituminous mixtures leave out volatile. These
volatile vapors contain hydro carbons [45]. So, they can catch the fire
easily and if further prone to heat the material may ignite and burn. By
the addition of CFA in BG-modified bitumen the flash and fire point are
increasing (Fig. 8).

3.2. Storage stability analysis

The softening point test is a common test for storage stability of

modified asphalt binder. The storage stability analysis is calculated in
terms of separation index SI, which is the difference of the softening
points between the top and bottom sections of the sample [40]. If the
difference is less than 2.2 ◦ C as per BS EN 13399:2017 [35], which is
defined as maximum permissible limit for validating homogeneous
dispersion of the blends. This study results shows that the SI values for
Fig. 8. Flash and fire point results.
neat binder and all four types of blends are below 2 ◦ C, which falls
within the specifying limits and satisfying proper storage stability
respectively. As the percentage of CFA increases the PI increases more (Fig. 9).
rapidly, which means that the BG and CFA modified bitumen is highly
resistive to temperature. The tensile properties of the asphalt binder
3.3. Moisture susceptibility analysis
were checked by performing ductility test. From the results it is
concluded that with the increasing amount of CFA in BG-modified
The moisture susceptibility of CFA and BG-modified bitumen were

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J. Muhammad et al. Construction and Building Materials 308 (2021) 125135

assessed from the following test results.

3.3.1. Bitumen bond strength test

The challenge to quantitatively evaluate the adhesive bond between
aggregates and modified asphalt binder is to identify a test that is simple,
quick and repeatable for evaluating adhesion properties of asphalt-
aggregates systems.
Youtcheff and Aurilio used the PATTI test, originally developed for
the coating industry to measures the moisture susceptibility of asphalt
binders [46]. For the bitumen bond strength test, a rectangular concrete
blocks specimen was used. The preparation of these blocks was done in
accordance to ASTM D 1985 [47].
The results of this study are presented in (Figs. 10 & 11). The
bitumen bond strength is shown in term of pull of tensile strength
(POTS) for 24 h dry and 24 h moisture conditioned. It’s concluded from
the results that with the addition of more CFA in BG modified bitumen
significantly improved approximately 28% of the POTS dry sample
Fig. 10. POTS values of dry samples. values, while for the moisture condition samples the increase is 14%
only. The increase in POTS values indicate the stronger tensile strength
of the modified binder, which is due to the addition of CFA in BG-
modified asphalt. From these results we can say that CFA performs
well in reducing the effect of moisture, but in comparison to dry samples
the increase in POTS values were 50% less. The POTS values for wet
sample is more than the neat binder but less than the dry sample because
the addition of CFA in BG-modified binder cannot completely eliminate
the moisture sensitivity of BG-modified asphalt.

3.3.2. Rolling bottle test

Another test to check the moisture susceptibility of loose coated
asphalt mixture sample is rolling bottle test [48]. The results are pre­
sented in (Fig. 12) which shows the comparison of remaining percentage
coating around aggregates of modified and unmodified asphalt binder at
duration of 6 h, 24 h, 48 h and 72 h. It is observed from the results that
percentage coating lost was slightly decreased with the addition of BG
and CFA. So, it’s concluded that CFA slightly reduced the moisture
susceptibility of BG-modified asphalt, not completely.
The binder-aggregate bond strength is stronger as compared to the
Fig. 11. POTS values of wet samples.
previous study by [49]. The increase in strength of binder-aggregate
bond strength is due to making blend of BG-modified asphalt with
different CFA parentages.

Fig. 12. Loss of coating for various CFA percentages at different durations.

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J. Muhammad et al. Construction and Building Materials 308 (2021) 125135

permanent deformation (Rutting etc.). If the dynamic modulus values

are high for an asphalt mixture so its permanent deformation resistance
is good and vice versa [50,51]. All tests were performed at 21 ◦ C and
38 ◦ C considering the climatic condition of China. It is concluded from
the results shown in (Figs. 13 & 14) that the dynamic modulus of asphalt
mixture increases with increase in loading frequency and decreases with
an increase in the test temperature [52]. Furthermore, it is observed that
the combination of 10% BG + 6% CFA shows better results of dynamic
modulus at both temperatures and frequencies.
The reason behind increment in dynamic modulus values with the
addition of BG and CFA are, it produces attractive forces between
asphalt binder and aggregates. These additives fill the gaps among ag­
gregates causing improvement in dynamic modulus values [53].

3.5. Fatigue life

3.5.1. Four-Point bending beam fatigue test

Fig. 13. Dynamic modulus graph at 21 ◦ C. Fatigue type of distress in flexible asphalt pavement is very common
in most of the areas in china due the cold weather/low temperature in
most regions of the country, where most of the times temperature rea­
ches below 0◦ [54]. This type of distress mainly effects the wearing
coarse of flexible asphalt pavement [55]. The fatigue resistance was
assessed in terms of loading cycles to failure and the test used is Four-
point bending beam fatigue test [56].
From Fig. 15 it is noted that loading cycles to failure increases as the
CFA percentages increases. The optimum values of loading cycles to
failure were noted at 10% BG + 6% CFA which is approximately 89.5%
more than the neat binder. Due to the addition of CFA in BG-modified
asphalt, the fatigue life can be increased up to considerable amount in
contrast with the control mixture.

4. Conclusions

The results of this study indicate that the combination of BG and CFA
is suitable for asphalt modification to increase its rheological and
mixture properties, these additives are also economical and environ­
mental friendly. The BG can be produced in any desirable quantity as it
Fig. 14. Dynamic modulus graph at 38 ◦ C. is produced from the animal wastes, which is a sustainable source and is
easily available in local market. The CFA can be easily obtained in the
3.4. Permanent deformation analysis market and is affordable comparing with other chemicals and additives.
The key conclusions of this research can be found as following:
3.4.1. Dynamic modulus test
This test is used to evaluate the resistance of asphalt mixture against (1) FTIR and storage stability analysis results show that the mixing
procedure employed for BG and CFA in asphalt binder is suitable

Fig. 15. Fatigue life of BG and CFA modified asphalt mixture at 25 ◦ C.

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J. Muhammad et al. Construction and Building Materials 308 (2021) 125135

and showing the complete dispersion of BG and CFA particles and [4] M. Liang, S. Ren, W. Fan, X. Xin, J. Shi, H. Luo, Rheological property and stability
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