Effect of Nanoclay on Physical and Rheological Properties

of Waste Cooking Oil–Modified Asphalt Binder

Nikhil Saboo 1; Mayank Sukhija 2; and Gaurav Singh 3
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Abstract: The use of waste cooking oil (WCO) and nanoclay (NC) in the modification of asphalt binder can produce sustainable material for
paving applications. This study evaluated the change in physical and rheological properties attained by modification of a conventional asphalt
binder using varying percentages of WCO and NC; 0%, 2.5%, and 5% WCO was used to modify a VG 30 binder, followed by reinforcement
using four different dosages of montmorillonite NC (0%, 2%, 4%, and 6%). A total of 12 combinations of asphalt binders were produced
(VG30, 2NC, 4NC, 6NC, 2.5WCO, 5WCO, 2.5WCO2NC, 2.5WCO4NC, 2.5WCO6NC, 5WCO2NC, 5WCO4NC, and 5WCO6NC) and
subjected to physical (penetration, softening point, viscosity, and temperature susceptibility) and rheological [high-temperature performance
grading (PG), multiple stress creep and recovery (MSCR), and linear amplitude sweep test (LAS)] measurements. The physical and rheo-
logical measurements showed that the use of NC in WCO-modified asphalt binder could reverse the softening effect caused by the inclusion
of WCO in VG 30. At 50°C and 60°C, 2.5WCO with 4% and 6% NC had higher values of percentage recovery (R) compared with VG 30.
It was found that the use of NC insignificantly increased the strain susceptibility of the asphalt binders at intermediate temperatures for all
WCO levels. Statistical analysis revealed that the effect of modification on unrecoverable creep compliance is less significant than the change
in R for a temperature range of 40°C–70°C. The significance of modification at intermediate temperatures was not consistent and clear.
A simple cost–benefit analysis was proposed, which indicated that 2.5WCO6NC is the optimum combined blend for obtaining higher bene-
fits relative to the cost of modification. DOI: 10.1061/(ASCE)MT.1943-5533.0003598. © 2020 American Society of Civil Engineers.
Author keywords: Waste cooking oil (WCO); Nanoclay (NC); Asphalt binder; Multiple stress creep and recovery (MSCR); Linear
amplitude sweep test (LAS).

Introduction
Hot-mix asphalt (HMA), which acts as the surface layer in flexible
pavements, is a combination of mineral aggregates and asphalt
binder mixed in a certain proportion and compacted to the required
density (Choudhary et al. 2019; Pouranian and Haddock 2019).
Asphalt binder, which comprises approximately 10%–12% of the
total volume, is the most important and costliest component of
HMA. It is a viscoelastic material obtained through the frac-
tional distillation of crude oil, a nonrenewable source of energy
(Whiteoak 1990). Environmental regulations and economic con-
cerns have compelled researchers to explore alternative and sustain-
able sources of binder in HMA (Aziz et al. 2015; Pouranian and
Shishehbor 2019). The result of this search for an alternate material
has led to the development of an ecologically viable binder called
bioasphalt (BA). BA produced from biowaste and biomass has been
studied by various researchers (Al-Sabaeei et al. 2019; Fini et al.
2010; Ingrassia et al. 2019; Sun et al. 2017; Wang et al. 2018). BA
derived from multiple sources, including manure, swine, oakwood,
1 (Azahar et al. 2016a). In general, the use of waste cooking oil in
Assistant Professor, Dept. of Civil Engineering, Indian Institute of
Technology, Varanasi, Uttar Pradesh 221005, India. Email: nikhilsaboo
.civ@iitbhu.ac.in
2
Research Scholar, Dept. of Civil Engineering, Indian Institute of
Technology, Varanasi, Uttar Pradesh 221005, India (corresponding author).
Email: mayanksukhija.rs.civ18@itbhu.ac.in
3
M.Tech. Student, Dept. of Civil Engineering, Indian Institute of
Technology, Varanasi, Uttar Pradesh 221005, India, Email: gauravsingh
.civ18@itbhu.ac.in
Note. This manuscript was submitted on April 18, 2020; approved on
August 3, 2020; published online on December 23, 2020. Discussion per-
iod open until May 23, 2021; separate discussions must be submitted for
individual papers. This paper is part of the Journal of Materials in Civil
Engineering, © ASCE, ISSN 0899-1561.
and waste cooking oil (WCO), has proved to be a useful alternative
to conventional asphalt binder (Warith and Khedr 2013; Fini et al.
2010; Maniruzzaman et al. 2016; Wen et al. 2013; You et al.
2011a).
WCO, obtained from households, restaurants, and other food in-
dustry sources, is in abundance (Asli et al. 2012). About 15 million
tons WCO is generated annually (Gui et al. 2008). Out of the total
available WCO, the US produces approximately 10 million tons/
year. European countries, Canada, the United Kingdom, and Japan
generate about 0.7–1 million tons, 0.135 million tons, 0.2 million
tons, and 0.45–0.57 million tons/year WCO, respectively. On the
other hand, China, a country with high population density, generates
about 4.5 million tons/year. The lowest annual production of WCO
is recorded in Ireland, about 0.153 million tons. In India, the exact
amount of generated WCO is not available. According to reports of
2009–2010 oil consumption, about 0.167 million tons WCO is an-
ticipated (Panadare and Rathod 2015). Such a huge production of
WCO is presumed to increase at a rate of 2% per year, which can
create problems related to its collection, treatment, and disposal
HMA has been explored through two different utilities: as a BA after
polymerization, or as a softening agent for reclaimed asphalt pave-
ment (RAP) (Behnood 2019; Zargar et al. 2012). Previous works
have reported that WCO-modified asphalt binders are softer and
exhibit lower viscosity (Bilema et al. 2019; Chen et al. 2014;
Cong et al. 2020). The quality of the WCO also influences the per-
formance of the modified blend (Adesina and Dahunsi 2020).
Azahar et al. (2016b), studied the effect of the use of untreated
and treated WCO on the properties of asphalt binder and reported
that the acid content of WCO is critical in affecting the performance
of HMA. The use of untreated WCO has been found to reduce
the viscosity of base asphalt binder and can be detrimental to the

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 rutting performance. Sun et al. (2016) revealed that physical inter-
action occurs upon mixing WCO with the asphalt binder. They
found that the intermixing of WCO decreases the deformation re-
sistance of control asphalt binder. Owing to the improved low-
temperature performance of WCO-inclusive asphalt binder, it can
be utilized as an asphalt alternative for cold regions (Al-omari
et al. 2018; Joni et al. 2020). Similar results were reported by
Maharaj et al. (2015b) and Wen et al. (2013), who found increased
resistance to fatigue distress at low temperatures. Those studies also
concluded that intermixing of WCO in the asphalt binder results in
low rutting resistance at elevated temperatures. Analogous results
were reported in a few other studies (Gong et al. 2016; Ji et al.
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2017; Maharaj et al. 2015a; Xinxin et al. 2018). It is expected that
the use of viscosity enhancers, in addition to WCO, can improve the
performance of WCO-modified asphalt binder.
Although many state-of-the-art technologies have evolved for
the modification of asphalt binders, the use of nanotechnology-
based modification is very effective (Fang et al. 2013; Jamshidi
et al. 2015; Yao et al. 2013a, b). Nanotechnology has the capability
to reinforce and improve the properties of asphalt binder at the mi-
crolevel as well as the macrolevel (Mills-Beale and You 2011;
Azahar et al. 2015; Yang and Tighe 2013). Nanoclay (NC), a subset
of nanotechnology, has been accepted widely for ameliorating the
performance of asphalt binders. NC has a low production cost and
is abundantly available in nature. Its efficiency in alleviating the
mechanical response of asphalt binders makes NC a productive
modifier (Ezzat et al. 2016; Hossain et al. 2015; Zilg et al. 2001).
Ghanoon et al. (2020) found that the addition of NC in asphalt
binder improves the temperature susceptibility and reduces the
stress sensitivity at the tolerance temperature (64°C). Wu et al.
(2010) found that the use of NC is an effective way to ameliorate
the overall performance of asphalt binder. You et al. (2011b)
explored different types of NC and found that irrespective of NC
type, its addition in asphalt binders influences the rheological per-
formance with an increase in viscosity. Various types of NCs are
available for modifying asphalt binder, e.g., kaolinite (Zhu et al.
2014), vermiculite, montmorillonite (Bonati et al. 2013), hectorite
(Silvestre et al. 2016), and saponite (Ray and Okamoto 2003).
Among the aforementioned types of NC, montmorillonite com-
monly has been used in practice due to its nontoxicity and excellent
biocompatibility (Lakshmi et al. 2010).
Although the use of WCO can help in replacing the quantity of
asphalt binder for paving applications, there are concerns regarding
reduction in stiffness, which may lead to the occurrence of perma-
nent deformation. The use of modification to compensate for the
loss of stiffness is an interesting area of study. Although the use
of WCO has been explored previously, its use as a direct replace-
ment for asphalt binders has not been explored with enough rigor.
This forms the motivation for the present work. This study had two
objectives: (1) to study the effect of direct replacement of WCO in
asphalt binder, and (2) to find a suitable NC dosage to add to WCO-
modified asphalt binders to obtain satisfactory performance in
terms of rutting and fatigue. To achieve these objectives, different
combinations of WCO- and NC-modified asphalt binders were
studied using physical and rheological measurements in a temper-
ature range of 10°C–70°C. To the best knowledge of the authors, no
previous studies have reported the use of NC in combination with
WCO in asphalt binders. It is expected that this combination will
lead to the development of a sustainable alternate binder with better
performance in terms of rutting and fatigue. This also will lead
to the replacement of crude oil–derived asphalt binder using an
ecologically sound approach and environmentally friendly technol-
ogy. A cost–benefit study, in addition to statistical analysis, proved
the efficiency of NC-inclusive WCO-modified asphalt binder.
© ASCE 04020490-2
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The results of this study can be used by researchers and practi-
tioners to understand and assess the suitability of NC in improving
the performance of WCO-modified asphalt binder.
Materials
Asphalt Binder
One viscosity-graded (VG) asphalt binder, VG 30, was used in this
research work as the control binder for fabricating all the modified
asphalt blends. The number 30 in VG 30 indicates that the dynamic
viscosity of the binder at 60°C ranges from [30 × 100 ± 80 Pa·s to
30 × 100 ± 60 Pa·s (30 × 100 ± 800 Poise to 30 × 100 ± 600
Poise)]. VG 30 was collected from a single source to certify the
consistency of original binder characteristics.
Waste Cooking Oil
Generally, the disposal of WCO into landfills or nearby rivers has a
negative impact on the environment. Hence, proper management of
disposal activities has become a question of great concern world-
wide. WCO used in this study was obtained from a roadside res-
taurant at no cost. It was a typical unsaturated plant-based oil that is
liquid at ambient temperatures. The procured raw WCO contained
various suspended waste particles that were screened using a sim-
ple filtering procedure. WCO was allowed to pass through a filter
paper to remove undesirable fried particles.
Nanoclay
This study used a powdered form of montmorillonite NC, com-
posed of organically modified phyllosilicates. In general, montmo-
rillonite is a member of the smectite family, with a 2∶1 layered
structure with one octahedral sheet intercalated between two tetra-
hedral sheets (Liu et al. 2011). The NC used in this study was pur-
chased from a private manufacturer. Table 1 presents the typical
properties of NC used in this study.
Fabrication of Modified Blends
To prepare the modified asphalt binder, the mixing process was
performed in two phases. VG 30 was heated using a temperature-
controlled heating mantle until it was fluid enough to be poured.
Subsequently, 500 g binder was put in a separate container and
stirred properly to eliminate air bubbles. Predetermined dosage of
WCO (2.5% and 5% by weight of binder) were added to the pre-
heated asphalt binder. Initially, manual mixing was performed us-
ing a glass rod for 20 min, followed by mixing with a low-shear
stirrer. The stirrer was operated at a speed of 500 rpm for 30 min
to attain homogeneous dispersal of WCO in the base asphalt binder.
In the second phase, predefined contents of NC (2%, 4%, and
6% by weight of binder) were added to the control asphalt binder
and WCO-modified asphalt binder. Mixing was done using a
Table 1. Typical properties of NC
Serial number Property Specified value
1 Composition Organophyllosilicates
2 Bulk density (kg=m3 ) 130
3 Water content (%) <6
4 Specific weight (g=cm3 ) 1.5–1.7
5 Particle size (μm) <10
6 Platelet thickness (nm) <80
7 Color Off-white
J. Mater. Civ. Eng.

similar protocol, with a high-shear mixer operated at 4,000 rpm.
A total of 12 combinations were prepared and the samples were
named as follows: VG30 (base asphalt binder), 2NC (2% NC þ
VG30), 4NC (4% NC þ VG30), 6NC (6% NC þ VG30), 2.5WCO
(2.5% WCO þ VG30), 5WCO (5% WCO þ VG30), 2.5WCO2NC
(2.5% WCO þ 2% NC þ VG30), 2.5WCO4NC (2.5% WCO þ 4%
NC þ VG30), 2.5WCO6NC (2.5% WCO þ 6% NC þ VG30),
5WCO2NC (5% WCO þ 2% NC þ VG30), 5WCO4NC (5% WCO þ
4% NC þ VG30), and 5WCO6NC (5% WCO þ 6% NC þ VG30).
A small amount of asphalt binder from each combination was
subjected to short-term aging (STA) and long-term aging (LTA)
using the Universal Simple Aging Test (USAT) procedure devel-
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oped by Western Research Institute (WRI) (Farrar et al. 2012).
USAT uses a draft oven to age the asphalt binder, and has been
successfully adopted and reviewed in various other studies (Kriz
et al. 2017; Saboo and Sukhija 2020; Wang et al. 2015, 2016).
Asphalt binders in the unaged condition, STA condition, and
LTA condition were stored in separate containers for supplementary
investigation. All the tests were performed three times, and the
average of the obtained results are presented in this study. It was
found that the coefficient of variation for all the measurements was
less than 10%.
Experiment
Conventional Tests of Asphalt Binders
To assess the effect of WCO and NC on the physical properties of
VG 30, conventional tests, including penetration (pen), softening
point, and viscosity, were carried out. The results of the physical
tests were used to calculate the temperature susceptibility (TS) of
the asphalt binders. Penetration index (PI) was used to evaluate TS
for different combinations of WCO-NC–modified binders. The PI
is a quantitative measure of the response of bitumen to variation in
temperature. The best known method is that developed by Pfeiffer
and Van Doormaal (Whiteoak 1990), which can be mathematically
written as follows:
20ð1 − 50TSÞ
PI ¼ ð1Þ
1 þ 50TS
where TS = temperature susceptibility, which is the slope of the
graph of the logarithm of penetration to temperature. Assuming that
the penetration of most asphalt binders is 800 dmm at its softening
point, TS can be calculated as follows:
log penT 1 − log 800
TS ¼ ð2Þ
T 1 − softening point
Taking the penetration value at 25°C, Eqs. (1) and (2) can be
combined as:
1952 − 500 log pen − 20 softening point
PI ¼ ð3Þ
50 log pen − softening point − 120
This study used Eq. (3) to assess the temperature sensitivity of
the asphalt binders.
Multiple Stress Creep and Recovery
The high-temperature performance of asphalt binders can be
studied using the multiple stress creep and recovery (MSCR)
test. This study conducted MSCR tests using a dynamic shear
rheometer (DSR) as per the details outlined in AASHTO T 350
© ASCE 04020490-3
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Jnr= ur/ 0 ; R = [ r/( ur+ r)].100
0.012
0.01
Strain, mm/mm
0.008
0.006
0.004
0.002
0
0 2 4 6 8 10 12
Time, Sec
Fig. 1. Schematic representation of creep and recovery. (Data from
Saboo and Kumar 2016.)
(AASHTO 2014c). STA samples were used with a 25-mm spindle
and a 1-mm gap setting in the DSR. As per the standard specifi-
cation, the asphalt binder is subjected to a consecutive cycle of 1-s
creep and 9-s recovery at stress levels of 0.1 and 3.2 kPa, respec-
tively. The cycles are continuous, with 10 cycles at each stress level.
The measurements are recorded after 10 conditioning cycles at
0.1 kPa. This is done to obtain stable readings during the test.
MSCR tests in this study were conducted at 40°C, 50°C, 60°C,
and 70°C on all the asphalt binders. The measured response was
used to calculate the nonrecoverable creep compliance (J nr ) and
percentage recovery (R) averaged over the 10 cycles; J nr and R
can be used to quantify the rutting susceptibility of asphalt binders.
A typical schematic response obtained in MSCR test along with the
calculation of J nr and R is presented in Fig. 1.
Linear Amplitude Sweep
The fatigue life of asphalt binders can be evaluated using linear
amplitude sweep (LAS) test in a very short period. The viscoelastic
continuum damage (VECD) principle is used to derive the damage
characteristics of binders subjected to continuous increasing strain
amplitude. A DSR was used with LTA samples to perform the LAS
test using an 8-mm-diameter spindle with a 2-mm gap setting. The
experiment was performed as per AASHTO TP 101-14 (AASHTO
2014a) to determine parameters A and B, in the asphalt binder
fatigue equation
N F ¼ Aðγ max ÞB ð4Þ
First, a frequency sweep test is conducted at a low strain am-
plitude of about 0.1%, to obtain an undamaged material property,
α, which is used to calculate parameter B in Eq. (4) (B ¼ −2α).
This is followed by an amplitude/strain sweep test conducted at
a frequency of 10 Hz, with a linearly increasing load amplitude
from 0.1% to 30% in 300 s. The amplitude is increased at a rate
of 1%, subjecting the binder to 100 cycles at each strain value. This
step is used as an input in viscoelastic continuum damage analysis
to determine A.
Results and Analysis
Physical Test Results
Table 2 presents the results of physical tests done on various asphalt
binders along with the value of temperature susceptibility and
penetration index. The inclusion of NC in VG 30 increased its
J. Mater. Civ. Eng.
 Table 2. Physical properties of asphalt binders NC in WCO-modified asphalt binders, the temperature susceptibil-
Penetration Softening ity decreased. The rate of decrease in temperature susceptibility
value point Viscosity at with increase in the dosage of NC was higher in 5% WCO–
Binder type (dmm) (°C) 60°C [Pa·s (P)] TS PI modified binders than in 2.5% WCO–modified asphalt binders.
VG 30 68 50 271.2 (2,712) 0.0428 −0.449 This indicates a thermomechanical interaction between WCO and
2NC 40 56 290.6 (2,906) 0.0419 −0.317 NC which is more significant at higher dosage of WCO. Further-
4NC 35 60 369.6 (3,696) 0.0388 0.199 more, 2.5% WCO–modified binder with 6% NC (2.5WCO6NC)
6NC 31 65 463.9 (4,639) 0.0352 0.851 had physical behavior similar to that of the control binder (Table 2).
2.5WCO 97 46 145.4 (1,454) 0.0436 −0.571 Thus, the use of WCO in combination with NC can be effective for
2.5WCO2NC 85 50 188.2 (1,882) 0.0389 0.178 use in paving applications.
2.5WCO4NC 74 54 230.0 (2,300) 0.0356 0.781 An attempt was made to correlate the physical properties. The
2.5WCO6NC 66 59 258.0 (2,580) 0.0318 1.567
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best-fit equation with the corresponding coefficient of correlation

5WCO 134 40 81.2 (812) 0.0517 −1.635
5WCO2NC 125 44 106.6 (1,066) 0.0424 −0.389
(R2 ) is presented in Figs. 2(a–d). The horizontal and vertical error
5WCO4NC 109 50 179.5 (1,795) 0.0346 0.983 bars indicate reasonable repeatability of the test results. It was
5WCO6NC 98 54 243.2 (2,432) 0.0314 1.663 found that penetration, viscosity, and softening point had appreci-
able intercorrelations, whereas the temperature susceptibility could
not be correlated with any physical parameter [e.g., the graph of
viscosity versus TS is presented in Fig. 2(d)].
viscosity and softening point, and decreased its penetration. NC
modification also led to a reduction in temperature susceptibility
High-Temperature PG Grading
with the increase in the value of PI. This indicates a positive impact
of NC modification. Inclusion of WCO in VG 30 had the opposite AASHTO M 320 (AASHTO 2017) was used to obtain the high-
effect. The percentage reduction in viscosity and softening point temperature performance grade (PG) of all the asphalt binders.
for 2.5WCO was 46% and 8%, respectively, whereas for 5WCO The high temperature PG grade is the maximum temperature at
it was 70% and 20%. The corresponding increase in penetration which the value of G=sin δ in unaged and STA conditions is more
was 42% and 97%, respectively. The inclusion of NC in WCO- than 1 and 2.2 kPa, respectively. The value of the PG tempera-
modified binders compensated for this loss in viscosity. The high ture usually is checked at a difference of 6°C. In addition to the
specific surface area of nanoclay can improve the physical network high-temperature PG grade, the true fail temperature (the actual
within the asphalt matrix, which leads to an increase in stiffness temperature beyond which the asphalt binders fails to meet the de-
(Abdelrahman et al. 2014). The addition of WCO increased the sired criteria) was evaluated. Table 3 presents the corresponding
temperature susceptibility of VG 30 by 2% and 20% for 2.5% values for all the asphalt binders. With an increase in the percentage
and 5% WCO, respectively. With an increase in the dosage of of NC for different WCO dosages, the PG grading increased.

(a) (b)

(c) (d)

Fig. 2. Correlations between different physical parameters of WCO and NC modified asphalt binders: (a) penetration value and viscosity;
(b) softening point and viscosity; (c) softening point and penetration value; and (d) temperature susceptibility and viscosity.

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 Table 3. High-temperature PG grade of asphalt binders
NC
0% 2% 4% 6%
True fail True fail True fail True fail
temperature High-temperature temperature High-temperature temperature High-temperature temperature High-temperature
WCO (%) (°C) PG grade (°C) PG grade (°C) PG grade (°C) PG grade
0 74.3 PG 70 76.5 PG 76 77.5 PG 76 80.4 PG 76
2.5 72.6 PG 70 75.8 PG 70 77.0 PG 76 79.8 PG 76
5 61.9 PG 58 65.6 PG 64 67.7 PG 64 70.6 PG 70
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Although 2NC, 4NC, and 6NC had the same high-temperature PG
grade (for example, in case of 0% WCO), the true fail temperature
(Table 3) increased with an increase in NC. With an increase
in the percentage of WCO, the high-temperature PG grade de-
creased, and so did the true fail temperature. This is attributed
to the lower viscosity of the waste cooking oil. Addition of
NC to the WCO-modified asphalt binders reversed the decrease
of viscosity. The rate of increase in the true fail temperature with
the increase in NC at both WCO levels was higher than that
corresponding to 0% WCO. This agrees with the results obtained
for the TS characteristics of the modified asphalt binders. For
5WCO, a NC dosage of 6% produced a high-temperature PG
grade similar to that of VG 30. For 2.5WCO, the high-temperature
PG grade of the base binder (i.e., VG 30) improved from PG 70 to
PG 76 with of 4% and 6% NC. This demonstrates the stiffening
effect of NC, which can be beneficial for WCO-modified asphalt
binders.
Permanent Deformation Characteristics of Asphalt
Binders
As mentioned previously, MSCR tests are carried out at stress lev-
els of 0.1 and 3.2 kPa. Previous studies compared the values of J nr
and R of asphalt binders at a stress level of 3.2 kPa (Saboo et al.
2018; Saboo and Kumar 2015). This is due to the better correlation
obtained between the observed rut depth in pavement and the afore-
mentioned parameters obtained from MSCR tests at 3.2 kPa
(D’Angelo 2009; Narayan et al. 2019; Saboo and Kumar 2016).
The present study also compared the rutting performance of asphalt
binders only at 3.2 kPa. However, the discussions for 3.2 kPa are
applicable for 0.1 kPa as well. For brevity, the results and discus-
sion of the 0.1-kPa stress level are not provided.
Fig. 3 shows the variation of J nr at each temperature correspond-
ing to the change in the percentage of WCO and NC. In general, it
was found that, irrespective of temperature, the unrecoverable creep

Fig. 3. Variation of Jnr for asphalt binders at (a) 40°C; (b) 50°C; (c) 60°C; and (d) 70°C.

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(a)
(c)
Fig. 4. Variation of R for asphalt binders at (a) 40°C; (b) 50°C; (c) 60°C; and (d) 70°C.
compliance increased with an increase in the proportion of WCO,
which is attributed to the softening of the binder caused by the ad-
dition of waste cooking oil. With an increase in the percentage of
NC, the value of J nr decreased at all the WCO contents. The hori-
zontal line in Fig. 3 compares the value of unrecoverable creep
compliance of the base binder with those of the modified binders.
This helps to find the appropriate combination of WCO and NC
with similar rutting resistance to that of VG 30. Mixture 2.5WCO
when modified with 6NC had identical or better rutting perfor-
mance at all temperatures above 40°C. With an increase in temper-
ature, the difference between J nr of VG 30 and 2.5WCO6NC
increased, with the latter having better performance. This is
attributed to the reduction in viscosity of VG 30 with the increase
in temperature and the reinforcing effect of NC at higher
temperatures.
The analysis of percentage recovery (Fig. 4) produced interest-
ing results. It was found that the change in values of R with an
increase in the percentage of NC and WCO was more pronounced
compared with that of J nr . The value of R for VG 30 decreased
steeply with the rise in temperature. NC modification (both with
and without WCO) imparted elasticity to the binder, as is evident
from the increase in values of R (even at 70°C). At 50°C and 60°C,
2.5WCO with 4% and 6% NC had higher values of percentage
recovery than did VG 30. At 70°C except for 4NC, 6NC, and
© ASCE
J. Mater. Civ. Eng., 2021, 33(3): 04020490
(b)
(d)
2.5WCO6NC, the value of R for was 0. Asphalt binder, being
viscoelastic, loses viscosity with an increase in temperature. At
higher temperatures, the binder phase in the NC-modified binder
softens, but the NC phase retains the elasticity, improving the
rutting resistance of the binder. WCO, which is liquid even at
ambient temperatures, softens the base asphalt binder in general
but does not impact its rheological response with an increase in
temperature.
Fig. 5 shows the effect of temperature on the rutting resistance
of asphalt binders. With an increase in temperature, J nr decreased
for all combinations of NC and WCO. In general, no significant
difference in temperature susceptibility was observed between
unmodified and WCO/NC-modified binders. However, with the in-
crease in the percentage of NC, the values of J nr for WCO-modified
binders were closer to that of VG 30. This behavior was more
prominent at 70°C, especially for 2.5WCO6NC binder. This is
attributed to the softening of VG 30 and the stiffening effect of NC
at higher temperatures.
AASHTO M 332 (AASHTO 2014b) outlines the suitability of
asphalt binders for different traffic conditions based on the maxi-
mum value of J nr at 3.2 kPa. Traffic is categorized as standard (S),
heavy (H), very heavy (V), and extremely heavy (E). The corre-
sponding maximum desirable values of J nr are 4.5, 2, 1, and
0.5 kPa−1 , respectively. To adjudge the applicability of the asphalt
04020490-6 J. Mater. Civ. Eng.
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(a) (b)

(c) (d)

Fig. 5. Effect of temperature on J nr values for asphalt binders (a) 0% NC; (b) 2% NC; (c) 4% NC; and (d) 6% NC.

binders used in this study, a suitability chart was produced at each with 6% NC (i.e., 2.5WCO6NC) met the requirement for extremely
temperature using Table 4. The suitability pertains to different high traffic loadings. At 50°C, the modified asphalt binder with
traffic levels for which the respective binders can be used based on 5WCO6NC was found to be suitable for the V traffic category,
the specifications proposed in AASHTO M 332. At 40°C and 50°C, whereas other NC combination with 5WCO (at any other temper-
VG 30, with all combinations of NC (0%–6%) was found to be ature) satisfied the requirement for heavy traffic conditions. At
suitable for extremely heavy traffic conditions. At 40°C, all the 60°C and 70°C, none of the asphalt binders was found to be suitable
combinations of WCO also were found to be appropriate for E for extremely heavy loading conditions. At 70°C, VG 30 reinforced
traffic levels. However, at 50°C, only 2.5% WCO in combination with 2%, 4%, and 6% NC met the criterion required for standard
loading. The use of WCO at 70°C for <10 million standard axle
(msa) traffic is possible only with 2.5WCO6NC. Hence 2.5%
Table 4. Suitability of various binder combination for different traffic
WCO is the optimum dosage when combined with 6% NC for lo-
levels cations with high temperatures and standard loading conditions.
Temperature (°C)
Fatigue Resistance of Asphalt Binders
Oil (%) 40 50 60 70
The values of A and B (−2α) are used to quantify the fatigue behav-
0% NC
0 E E H NS ior for the asphalt binders using a linear amplitude sweep test,
2.5 E V S NS where A is a function of damage, and B represents the undamaged
5 E H S NS material property. The evolution of stress versus strain in the am-
plitude sweep test can be used as an essential tool to study the dam-
2% NC age induced in asphalt binders. Fig. 6 presents the variation of shear
0 E E H S
stress versus shear strain for 2.5WCO at different NC contents.
2.5 E V H NS
5 E H NS NS With the increase in temperature, irrespective of NC dosage, the
peak stress decreased, and the strain at failure increased. The re-
4% NC duction in stress peak is attributed to the decrease in stiffness of
0 E E H S the binder, whereas the increase in failure strain indicates an im-
2.5 E V H NS provement of strain tolerance in the binder with an increase in tem-
5 E H NS NS
perature. This observation was found to be applicable for all the
6% NC asphalt binders used in this study, irrespective of WCO and NC
0 E E V S percentage. The change in value of peak strain or failure strain
2.5 E E H S did not follow any specific trend with the increase in rate of NC
5 E V S NS or with the shift in WCO content. Table 5 lists the values of A
Note: E > 30 msa (standing); V > 30 msa (slow-moving); H ¼ 10–30 msa; and B obtained for all the asphalt binders. With the increase in tem-
S < 10 msa; and NS = not suitable. perature, the value of A increased and the value of B decreased for

© ASCE 04020490-7 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2021, 33(3): 04020490

Downloaded from ascelibrary.org by Auckland University Of Technology on 12/23/20. Copyright ASCE. For personal use only; all rights reserved.

(a) (b)

(c) (d)

Fig. 6. Variation of shear stress and shear strain for 2.5% WCO at (a) 0% NC; (b) 2% NC; (c) 4% NC; and (d) 6% NC.

Table 5. Values of A and B obtained in LAS test

0% WCO 2.5% WCO 5% WCO
LAS
parameter NC (%) 10°C 20°C 30°C 10°C 20°C 30°C 10°C 20°C 30°C
A 0 1.67 × 104 2.66 × 104 3.21 × 104 2.23 × 104 3.49 ×104 3.70 × 104 2.97 × 104 3.86 × 104 3.14 × 104
2 1.29 × 104 1.93 × 104 3.12 × 104 1.90 × 104 3.82 × 104 4.03 × 104 1.84 × 104 3.61 × 104 5.12 × 104
4 5.26 × 103 1.47 × 104 2.60 × 104 2.19 × 104 3.03 × 104 4.21 × 104 2.26 × 104 3.71 × 104 5.27 × 104
6 7.33 × 103 1.23 × 104 2.63 × 104 9.76 × 103 1.89 × 104 2.55 × 104 1.68 × 104 2.29 × 104 3.25 × 104
B 0 −2.09 −1.91 −1.83 −2.03 −1.97 −1.76 −2.15 −1.99 −1.72
2 −2.06 −1.96 −1.86 −2.17 −2.05 −1.97 −1.99 −1.96 −1.92
4 −2.14 −2.05 −1.98 −2.33 −2.17 −2.15 −2.16 −2.09 −1.98
6 −2.33 −2.20 −2.25 −2.47 −2.30 −2.24 −2.25 −2.04 −1.95

all the asphalt binders, indicating an improvement in fatigue life.
No reliable conclusions could be drawn from the change in values
of A with the increase in WCO and/or NC. At a particular temper-
ature, no significant decrease or increase was observed in the values
of A between different binders. Hence it can be concluded that
WCO/NC modification has no substantial effect on the damage
characteristics of the base asphalt binder at intermediate tempera-
tures. The change in WCO dosage had no significant impact on the
values of B (Table 5). However, an increase in NC percentage led to
an increase in the value of B at all test temperatures. This can be
attributed to the increase in stiffness of the binder, increasing its
strain susceptibility. Nevertheless, this small increment will not af-
fect the fatigue life of the asphalt binders significantly.
Statistical Analysis
Table 6 lists the results of a two-way ANOVA calculated corre-
sponding to MSCR test parameters. This analysis was carried
out to quantify the influence of WCO and its corresponding
NC dosages. The results indicate not only that temperature
has a significant effect on R, but that NC influences the behavior
of both unmodified and WCO-modified asphalt binders. How-
ever, the effect of NC on the values of J nr was found to be
insignificant (Fcalculated < Fcritical ).As far as R value is concerned,
the addition of NC in 5WCO modified asphalt binder led to an
insignificant effect as indicated by the lower value of Fcalculated
(3.31) in comparison with Fcritical value (3.86). Although the
impact of WCO reduces the effect of NC, it had a significant
effect (Fcalculated ¼ 8.00) on the elastic response of 2.5WCO-
modified asphalt binder. The composite WCO-NC–modified
asphalt binder altered the rutting behavior of VG 30 asphalt
binder.
The results of two-way ANOVA to examine the impact of WCO
and their corresponding NC dosage on LAS test parameters are
listed in Table 7. Analysis of LAS tests confirmed that both NC
and temperature had a significant effect on the fatigue behavior

© ASCE 04020490-8 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2021, 33(3): 04020490

 Table 6. Two-way ANOVA results for MSCR test parameters
Binder type Parameter Source of variation SS df MS Fcalculated P-value Fcritical
VG30 R NC 79.35 3 26.45 10.16 0.00 3.86
Temperature 826.14 3 275.38 105.74 0.00 3.86
Error 23.44 9 2.60 — — —
Total 928.93 15 — — — —
J nr NC 0.32 3 0.11 3.09 0.08 3.86
Temperature 41.11 3 13.70 393.12 0.00 3.86
Error 0.31 9 0.03 — — —
Total 41.74 15 — — — —
2.5WCO R NC 110.52 3 36.84 8.00 0.01 3.86
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Temperature 479.64 3 159.88 34.70 0.00 3.86

Error 41.47 9 4.61 — — —
Total 631.62 15 — — — —
J nr NC 4.85 3 1.62 2.62 0.12 3.86
Temperature 83.97 3 27.99 45.29 0.00 3.86
Error 5.56 9 0.62 — — —
Total 94.38 15 — — — —
5WCO R NC 17.70 3 5.90 3.31 0.07 3.86
Temperature 136.94 3 45.65 25.60 0.00 3.86
Error 16.05 9 1.78 — — —
Total 170.68 15 — — — —
J nr NC 7.27 3 2.42 2.68 0.11 3.86
Temperature 316.91 3 105.64 117.04 0.00 3.86
Error 8.12 9 0.90 — — —
Total 332.30 15 — — — —

Table 7. Two-way ANOVA results for LAS test parameters

Binder type Parameter Source of variation SS df MS Fcalculated P-value Fcritical
VG30 A NC 207,379,158 3 69,126,386 17.39 0.00 4.76
Temperature 679,618,517 2 339,809,258 85.50 0.00 5.14
Error 23,845,817 6 3,974,303 — — —
Total 910,843,492 11 — — — —
B NC 0.19 3 0.06 31.94 0.00 4.76
Temperature 0.06 2 0.03 16.34 0.00 5.14
Error 0.01 6 0.00 — — —
Total 0.27 11 — — — —
2.5WCO A NC 426,159,733 3 142,053,244 15.17 0.00 4.76
Temperature 676,713,267 2 338,356,633 36.13 0.00 5.14
Error 56,182,467 6 9,363,744 — — —
Total 1,159,055,467 11 — — — —
B NC 0.30 3 0.10 54.92 0.00 4.76
Temperature 0.10 2 0.05 27.16 0.00 5.14
Error 0.01 6 0.00 — — —
Total 0.40 11 — — — —
5WCO A NC 311,393,333 3 103,797,778 1.79 0.25 4.76
Temperature 814,295,000 2 407,147,500 7.02 0.03 5.14
Error 347,891,667 6 57,981,944 — — —
Total 1,473,580,000 11 — — — —
B NC 0.05 3 0.02 2.24 0.18 4.76
Temperature 0.12 2 0.06 8.86 0.02 5.14
Error 0.04 6 0.01 — — —
Total 0.21 11 — — — —

of asphalt binder. However, the influence of NC was insignificant
(Fcalculated < Fcritical ) for 5% WCO–modified asphalt binder. In ad-
dition, the presence of NC in 2.5WCO-modified asphalt binder had
a significant impact on both A and B parameters. On the other hand,
for A, an increase in the dosage of WCO reduced the effect of
temperature, because Fcalculated decreased from 85.50 (VG 30) to
7.02 for 5WCO-modified asphalt binder. This indicates that the
presence of WCO improves the resistance against the damage
due to a change in temperature. For B, no such trend of a change
in Fcalculated was observed. Hence, this confirms the efficacy of
WCO- and WCO-NC–modified asphalt binder to change the
fatigue behavior of VG 30 asphalt binder.

© ASCE 04020490-9 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2021, 33(3): 04020490

 0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
HB
Cost–Benefit Analysis
In addition to producing better performance, any modification tech-
5WCO6NC nique must be economically viable. The aforementioned results in-
dicate that NC modification offers benefits in terms of rutting and
0.57
0.59
0.62
0.91
0.89
0.87
0.64
0.62
0.69
0.63
0.47
0.33
0.11
0.00
fatigue characteristics of WCO-modified asphalt binders. However,
the higher cost of NC may not provide an economical solution. There-
fore, a simple cost–benefit study was conducted to determine the eco-
nomic gain or loss obtained for various modified asphalt blends.
5WCO4NC

The MSCR test parameters were used to calculate R=J nr from

0.76
0.96
1.00
0.87
0.91
0.88
0.89
0.94
0.96
0.86
0.28
0.11
0.00
0.00
40°C to 70°C, whereas the A=B ratio obtained from LAS test data
was used from 10°C to 30°C. Evidently, these ratios should be as
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high as possible for improved performance in terms of rutting and

fatigue, respectively. Because all the parameters have different units
5WCO2NC

and ranges of magnitude, normalization using Eq. (5) was carried

0.62
0.93
0.97
0.81
0.85
0.85
1.00
1.00
1.00
1.00
0.21
0.04
0.00
0.00
out to remove value biases
V − minðV 0 sÞ
NV ¼ ð5Þ
maxðV 0 sÞ − minðV 0 sÞ
5WCO
1.00
1.00
0.59
0.87
0.86
0.76
0.91
0.82
0.91
0.85
0.22
0.07
0.00
0.00
where NV = normalized value for elected parameter (J nr , R, A,
and B); V = true value of corresponding parameter obtained from
the respective test; and minðV 0 sÞ and maxðV 0 sÞ = minima and
2.5WCO6NC

maxima among all values at a particular temperature, respectively.

0.33
0.49
0.48
1.00
1.00
0.99
0.23
0.24
0.26
0.26
0.87
0.85
0.95
1.00

This normalization technique yielded values from 0 to 1. The use of

0 in the denominator of a ratio yields undefined values. To remove
this constraint, a hypothetical binder (HB) was chosen with
J nr ¼ 0, R ¼ 0, A ¼ 0, and B ¼ 0. For this HB, nonzero values
of NV were generated for actual asphalt binders. NVs obtained
2.5WCO4NC

for all the asphalt binders corresponding to different parameters

0.74
0.78
0.80
0.94
0.94
0.96
0.25
0.33
0.38
0.41
0.66
0.39
0.22
0.00

are presented in Table 8.

The NV ratio of all the modified asphalt blends was calculated
relative to VG 30. HB was neglected during this calculation. The
NV ratios obtained were averaged over different temperatures
2.5WCO2NC

(Table 9). The undefined values at 70°C were due to 0% recovery

obtained for a few modified asphalt blends. The NC ratio thus was
0.64
0.99
0.77
0.88
0.89
0.88
0.36
0.35
0.42
0.45
0.47
0.29
0.04
0.00

averaged to 60°C.
Finally, a combined benefit (CB) value for all the modified as-
phalt binders was calculated by calculating the weighted mean of
the averages corresponding to rutting and fatigue criteria. A weight
2.5WCO

of 50% was given to each performance criterion. The obtained

0.75
0.90
0.70
0.82
0.85
0.78
0.45
0.47
0.57
0.57
0.36
0.14
0.00
0.00

results are presented in the third column of Table 10

CB ¼ 0.5 × Average 1 þ 0.5 × Average 2 ð6Þ
6NC
0.25
0.32
0.50
0.94
0.96
1.00
0.13
0.14
0.21
0.25
1.00
1.00
1.00
0.99
Table 8. NV of different asphalt binders at various temperatures

The cost per kilogram of all the asphalt binders was calculated
(Table 10). The cost of WCO was considered to be 0 because it was
obtained for free in this study. An approximate cost of Rs 50=kg
4NC
0.18
0.38
0.49
0.86
0.89
0.88
0.15
0.17
0.25
0.28
0.81
0.71
0.63
0.16

was assumed for VG 30. The per kilogram price of NC obtained

from a private company was Rs 3,000. The unit cost may vary de-
pending on the source and supplier, and the calculations presented
2NC
0.43
0.50
0.59
0.83
0.85
0.83
0.16
0.18
0.25
0.30
0.72
0.57
0.32
0.00

in this study would change accordingly. The combined cost (C) per
kilogram of all the modified asphalt binder blends was calculated as
follows:
VG 30
0.56
0.69
0.61
0.84
0.83
0.82
0.19
0.24
0.29
0.33
0.60
0.35
0.09
0.00

 
1 y%
C¼ × 50 þ × 3000 ð7Þ
ð1 þ x%Þð1 þ y%Þ ð1 þ y%Þ
Temperature

where x% = percentage of WCO by weight of VG 30; and y% =

(°C)
10
20
30
10
20
30
40
50
60
70
40
50
60
70

amount of NC by weight of WCO-modified asphalt binder.

Table 10 lists the cost–benefit (C=B) ratio obtained for different
levels of WCO and NC modification. Only 2.5% WCO in combi-
nation with 6% NC had a C/B of less than 1 (as shown in bold
Parameter,

value), indicating a higher benefit relative to the cost of the blend.

It is thus concluded that 2.5WCO6NC is the optimum dosage for
NV

J nr

modification.
B

R
A

© ASCE 04020490-10 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2021, 33(3): 04020490

 5WCO6NC

Undefined
Table 10. Cost–benefit analysis of NC-modified binders

0.93
0.80
0.95
0.90
0.23
0.36
0.53

0.37
Binder Cost (=kg) Cost ratio Benefit ratio C=B
VG 30 50 —
2NC 107.82 2.15 1.70 1.26
4NC 163.45 3.26 2.40 1.36
5WCO4NC

Undefined
6NC 216.97 4.33 4.09 1.06
1.31
1.27
1.52
1.37
0.10
0.08
0.00

0.06
2.5WCO 48.78 0.97 0.71 1.36
2.5WCO2NC 67.43 1.34 0.80 1.66
2.5WCO4NC 85.36 1.70 1.12 1.51
2.5WCO6NC 102.62 2.05 2.86 0.71
5WCO 47.61 0.95 0.71 1.33
5WCO2NC

Undefined 5WCO2NC 66.29 1.32 0.68 1.94

Downloaded from ascelibrary.org by Auckland University Of Technology on 12/23/20. Copyright ASCE. For personal use only; all rights reserved.

5WCO4NC 84.24 1.68 0.71 2.36

1.15
1.32
1.52
1.33
0.07
0.03
0.00

0.03
5WCO6NC 101.52 2.03 0.63 3.19
Note: Bold value signifies the value of C/B lower than 1. It indicates that
only 2.5% WCO in combination with 6% NC has a C/B of less than 1. All
other binders have C/B greater than 1.
Undefined
5WCO
1.72
1.40
1.04
1.39
0.08
0.06
0.00

0.04

The preceding C=B analysis did not consider low-temperature

cracking in the calculations. Although the framework proposed is
applicable to any performance study, the current analysis was lim-
ited to the results obtained corresponding to the rutting and fatigue
2.5WCO6NC

Undefined

performance of NC-inclusive WCO-modified asphalt binders.

0.49
0.59
0.65
0.58
1.20
2.49
11.75

5.15

Conclusions

This study assessed the suitability of using NC to enhance the

2.5WCO4NC

Undefined

physical and rheological properties of waste cooking oil modified

1.17
1.00
1.12
1.10
0.82
0.81
1.85

1.16

asphalt binder. In addition to the study of physical and rheological

properties of various asphalt blends, statistical analysis and cost–
benefit calculations were conducted to determine the efficacy of
modification. Overall, the study concluded that 2.5% of WCO in
combination with 6% NC gives the best results in terms of both
2.5WCO2NC

Undefined

performance and economic benefits. Specific conclusions of this

1.10
1.33
1.17
1.20
0.41
0.57
0.28

0.42

study are as follows:

a. Addition of NC to WCO-modified asphalt binders improves
the physical and rheological properties. For high-temperature
PG grading and resistance to rutting, 2.5WCO in combina-
tion with 4% and 6% NC is recommended.
Undefined
2.5WCO

b. LAS tests gave mixed results, with no conclusive effect of

1.37
1.27
1.20
1.28
0.26
0.21
0.00

0.15

adding NC to WCO-modified asphalt binders on the fatigue

resistance of asphalt binders. The use of NC increased the
strain susceptibility of the WCO-modified blends.
c. The use of NC had an insignificant effect on the values of J nr
Undefined

according to the statistical analysis. However, the percentage

0.39
0.40
0.67
0.49
2.41
4.83
15.86

7.70
6NC

recovery was highly influenced by the modification. The stat-

istical analysis revealed that modification had a significant
effect at higher temperatures compared with that at inter-
mediate temperatures.
Table 9. NV ratios at different temperatures

Undefined

d. A simple cost–benefit analysis was conducted. The analysis

4NC
0.31
0.51
0.75
0.52
1.71
2.92
8.21

4.28

concluded that 2.5% WCO with 6% NC gives the best results

with a higher benefit relative to the cost of modification.
e. Microstructural analysis of the modified asphalt binder
blends was not performed in this study. The physical and
Undefined

rheological test results indicated possible morphological in-

2NC
0.78
0.71
0.96
0.81
1.44
2.21
4.14

2.60

teractions between the base asphalt binder, WCO, and NC.

The results of this study can be explained better by con-
ducting a detailed microstructural examination.
Temperature

Data Availability Statement

Average 1

Average 2

All data, models, and code generated or used during the study
(°C)
10
20
30

40
50
60
70

appear in the published article.

© ASCE 04020490-11 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2021, 33(3): 04020490

 Acknowledgments
The authors thank Hindustan Colas Private Limited for providing
the asphalt binder used in this study. The authors also thank the
Ministry of Human Resource and Development (MHRD), India,
for their support.
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