Construction and Building Materials 249 (2020) 118630

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Construction and Building Materials

journal homepage: www.elsevier.com/locate/conbuildmat

Optimisation of liquid rubber modified bitumen for road pavements and

roofing applications
Ana Jiménez del Barco Carrión a, Ayad Subhy b, Maria Angeles Izquierdo Rodriguez c, Davide Lo Presti d,e,⇑
a
University of Granada, Spain
b
Pavement Design and Asset Management, Civil and Infrastructure, AECOM, Nottingham, United Kingdom
c
Danosa Eurofoam, Spain
d
Nottingham Transportation Engineering Centre (NTEC), University of Nottingham, United Kingdom
e
Department of Engineering, University of Palermo, Palermo, Italy

h i g h l i g h t s g r a p h i c a l a b s t r a c t

Cost effective optimisation of

modified bitumen with liquid rubber
for pavements and roofing
membranes is presented.

Design optimisation technique
allowed producing superior
bituminous binders.

LR improves the flexibility at low in-
service temperatures (using up to 50%
contents), while EBS improves
stiffness at high in-service
temperatures.

The Response Surface Methodology
was successfully used to optimise the
final blends also in terms of cost.

Analytical functions amongst the
design parameters have been derived
and here provided for future design
exercises.

The final properties were comparable
to Polymer Modified Binders.

a r t i c l e i n f o a b s t r a c t

Article history: Polymer Modified Bitumens (PMBs) are largely used for pavement and roofing membranes applications
Received 22 November 2018 with Styrene-Butadiene-Styrene Block copolymer (SBS) playing a major role in both markets despite its
Received in revised form 28 February 2020 constantly increasing price due to the rising demand for quality bitumen modifiers. On the other hand,
Accepted 29 February 2020
there is an increasing trend of recycling end of life tyres generating Recycled Tyre Rubber (RTR) at afford-
Available online 22 April 2020
able price. This investigation aims at engineering a modified bitumen with a combination of Liquid
Rubber (LR), a homogeneous blend of 50–70% RTR pre-processed in combination with heavy oils, and
Keywords:
a wax denominated Ethylene Bis Stearamide (EBS). In the first phase, the effect of LR and EBS was inde-
Liquid rubber
EBS
pendently characterised and compared to PMBs. Next, the Response Surface Methodology (RSM) was
Response surface methodology used to predict the response of different combinations of LR and EBS in terms of low and high tempera-
Recycled tyre rubber ture properties and cost, to then be optimised targeting conventional and rheological properties of PMBs

⇑ Corresponding author at: Nottingham Transportation Engineering Centre (NTEC), University of Nottingham, United Kingdom; Dipartimento di Ingegneria,Edificio 8,
Universitá degli studi di Palermo, Viale delle Scienze, 90128, Palermo, IT.
E-mail addresses: ajbc@ugr.es (A. Jiménez del Barco Carrión), davide.lopresti@nottingham.ac.uk, davide.lopresti@unipa.it (D. Lo Presti).

https://doi.org/10.1016/j.conbuildmat.2020.118630
0950-0618/Ó 2020 Elsevier Ltd. All rights reserved.
2 A. Jiménez del Barco Carrión et al. / Construction and Building Materials 249 (2020) 118630
SBS modified bitumen currently used in asphalt mixtures and roofing membranes in UK. As a result, an optimum combination of
Asphalt mixtures LR and EBS was found leading to a cost-effective modified bitumen comparable to PMBs. The work pro-
Roofing membranes vided also analytical functions that could be of use in further design exercises.
1. Introduction
Pavement engineering and roofing are the main area of bitumen
applications. In both, bitumen is exposed to extreme conditions
such as elevated temperatures, ultraviolet radiation, presence of
moisture, freeze–thaw cycles, etc., (including traffic loads in the
case of pavements). These conditions produce undesired distresses
in pavements and roofs which cause their deterioration. In order to
cope with these issues, materials are needed to have outstanding
properties. Binders for pavements are required to be soft and vis-
cous at low temperature to be able to relax stresses, while stiff
and elastic at high/intermediate temperatures to resist permanent
deformations and fatigue cracking [22]. Analogously, binders for
roofing are required to be hard at high temperatures but soft and
flexible at low temperatures [3].
To obtain materials with such properties, bitumen modification
with polymers has been undertaken for decades [15]. Polymer
Modified Bitumens (PMBs) are largely used for pavement and roof-
ing membranes applications, with thermoplastic elastomers such
as Styrene-Butadiene-Styrene Block copolymer (SBS) playing a
major role in both markets. In fact, manufacturing a compatible
complex system made of a bituminous matrix and SBS allows
obtain enhanced bituminous binders: more flexible at low service
temperatures and stiffer and more elastic at high service tempera-
tures. The global market of SBS is constantly increasing driven by
robust demand across several end-use markets and by the rising
demand for quality bitumen modifiers, hence its market price is
changing accordingly. On the other hand, there is an increasing
worldwide trend of recycling end of life tyres, and with these being
a waste it can be assumed that the price of recycled tyre rubber
(RTR) through ambient grinding will remain constant and low for
years to come. Thus, engineering a bituminous binder with compa-
rable properties to PMBs but with RTR in place of SBS, is an exam-
ple of a more sustainable engineering [25,42]. Recycled tyre rubber
modified bitumen are not at all a new technology and are used in
several countries world-wide [30,33]. In fact, RTR has shown good
potential as a bitumen modifiers in terms of performance and envi-
ronmental and economic benefits, which have made it a popular
alternative to thermoplastic elastomer such as Styrene-
Butadiene-Styrene (SBS) Block copolymer [39,37,5,35]. The modifi-
cation of bitumen with RTR increases its elasticity and decreases its
thermal susceptibility [27,14,38]. Therefore, RTR binders exhibit
improved resistance to rutting, fatigue and thermal cracking in
pavements engineering [23,20,40] and are able to resist higher
temperatures in roofing applications [28].
However, RTR modified bitumen still presents a main technical
issue: the lack of storage stability at high storage temperature
when used in high contents (>15%). This prevents the use of larger
amounts of modifiers, as well forcing manufacturers to adapt their
production plants and thus limiting the widespread use of this
technology [28,30,36]. Liquid Rubber (LR) was already used in pre-
vious studies as a possible solution to cope with this issue [11],
however only recent studies [32] proved that LR can help to signif-
icantly increase the amount of recycled tyre rubber content in a
modified bitumen (up to 35%). LR is a visibly homogeneous blend
of 50–70% RTR with heavy oils that has shown to greatly enhancing
bitumen elasticity while reducing its stiffness. This has been
shown to positively affect the low-temperature behaviour of bitu-
Ó 2020 Elsevier Ltd. All rights reserved.
men, however concerns with stiffness reduction at high-service
temperatures (for asphalt) were reported. Such reduction of stiff-
ness at high temperatures hinders the advantages of the use of
RTR modifier, hence to compete with PMBs, the final bituminous
blend needs to be engineered in a manner that allows improving
high-service temperature properties while holding the benefits of
LR modification. These conclusions drove us to Ethylene bis (stear-
amide) (EBS).
EBS is a waxy white organic compound widely used in roofing
to increase the stiffness and elasticity of bitumen. In pavement
engineering, Ziari et al. [41] found that the modification of bitumen
with EBS improves rutting resistance of asphalt mixtures. How-
ever, according to literature, its application in pavement engineer-
ing is still limited and its potential is still to be exploited.
Within this materials’ scope, this investigation aims at combin-
ing the advantages of LR at low temperatures and EBS at high tem-
peratures for pavement engineering and roofing applications. To do
this, the use of adequate methodologies, such as the Response Sur-
face Methodology (RSM), is essential to ensure the achievement of
consistent and optimised designs with several modifiers [24]. RSM
is a practical and useful statistical procedure to predict specific
responses of systems or materials based on experimental data. It
consists of three main steps: (1) definition of responses; (2) predic-
tion of responses by model fitting; (3) evaluation of the fitted mod-
els (Bezerra et al. 2008). RSM has been widely used as a tool for the
optimisation of bitumen modifiers content showing the capability
to provide adequate designs [7,18]; Moghaddam et al. 2015).
The objective of this paper is to present the optimisation of LR and
EBS as bitumen modifiers in order to obtain cost-effective bitumi-
nous binders with overall properties, over the whole useful temper-
ature interval, comparable (±10%) with two PMBs currently used in
UK for road pavement asphalt mixtures and roofing membranes.
2. Research approach, materials and methods
Fig. 1 illustrates the main stages undertaken in this study. The
first step was the selection of materials. As stated above, the pur-
pose of LR as a bitumen modifier was to improve the rheological
properties of bitumens at intermediate to low temperatures. The
EBS wax was selected to enhance the elasticity and increase stiff-
ness of bitumen at high temperatures to compensate the possible
issues due to using high contents of LR. In the first phase, the effect
of each modifier was independently characterised to identify
whether they can produce similar properties to PMBs that are com-
monly used in pavements or roofing. For this, three dosages of LR
and EBS were blended with the neat bitumen. In the second phase,
different combinations of LR and EBS were defined using Design
Expert 9.0.6.2 software, different responses were selected to study
the blends in terms of low and high temperature performance and
cost, and the experimental results were obtained. Applying the
RSM, the prediction laws for the responses were obtained. Finally,
the desirability functions for the responses were defined and the
optimum dosages of LR and EBS were identified.
2.1. Materials
For the purpose of this investigation, a neat bitumen was mod-
ified with LR and EBS. The neat bitumen was selected as a 40/60
 A. Jiménez del Barco Carrión et al. / Construction and Building Materials 249 (2020) 118630 3

Fig. 1. Research methodology.

penetration grade bitumen according to EN 12591 [8]. LR is a tech-
nology supplied by Innovators LLC in USA and obtained with a pro-
prietary process composed from a digestion tank, a main reactor
and a cooling unit. In the first two tanks the 8# fibre and glass free
RTR (2.36 mm) is subjected to a process of devulcanisation and
mixed with heavy oils derived from petroleum and/or soy. The pro-
cess is customisable, allows having control of the off gases, and has
a production rate of 12–25 Gal/h of LR. The end product is a sticky
visibly homogeneous fluid that varying the composition and pro-
cessing conditions can have different viscosities. The tested pro-
duct was labelled as Liquid Rubber (LR) and is composed of 50%
RTR + 50% of heavy oils. No other details of the production process
have been disclosed to the authors. EBS is a semi-synthetic wax (an
amide wax) produced by condensation of fatty acids and amines.
Two dosages of LR and EBS were firstly selected to be blended
with the neat bitumen in order to independently study the influ-
ence of each modifier on the neat bitumen properties. Two typical
SBS-PMBs commonly used in pavement engineering and roofing,
respectively, were used as control binders for comparison with
the blends. The conventional properties of these materials were
determined as a first characterisation and are shown in Table 1.
The softening effect of the LR and the hardening effect of EBS on
the neat bitumen can be observed.
2.1.1. LR/EBS and neat bitumen blends manufacturing
Rotational viscosity was the controlled physical parameter dur-
ing the modification process. Blends were manufactured in labora-
tory using a modified Brookfield Viscometer to operate at low-
shear mixing (100 rpm), and real-time viscosity measurements
were obtained under a controlled environment. The use of a mod-
ified impeller (dual helical impeller) allowed sample homogeniza-
tion during mixing [31].
For the LR blends, it has to be considered that when rubber and
bitumen are being blended, the viscosity of the blend increases up
to a maximum value (peak viscosity) and then suffers a noticeable
decrease with the reaction time. The maximum viscosity is recog-
nized as the peak of the modification process. In this investigation,
the peak viscosity was fixed at the point where the viscosity did
not increase more than 5% within 15 min [6]. After reaching the
peak viscosity, the mixing was continued for one hour in order to
ensure the stabilization of the properties of the blend having a final
blending time of 75 min. The LR blends were manufactured at

Table 1
Materials’ conventional properties.

Binder LR dosage (%) EBS dosage (%) Penetration (x0.1 mm) [9] Softening point (°C) [10]
Neat bitumen 0 0 46 87
PMB (roofing) 0 0 87 103
PMB (pavement) 0 0 55 91
Neat bitumen + 25% LR 25 0 76 49.6
Neat bitumen + 50% LR 50 0 136 44.2
Neat bitumen + 3% EBS 0 3 28 90.5
Neat bitumen + 6% EBS 0 6 28 111
4 A. Jiménez del Barco Carrión et al. / Construction and Building Materials 249 (2020) 118630

180 °C. In the case of EBS blends, the reaction time was 60 min and
the blends were manufactured at 150 °C.
2.2. Research phases
2.2.1. Phase I: Individual influence of modifiers
The individual influence of modifiers was characterised by
means of their Linear Visco-Elastic (LVE) properties. For this, rheo-
logical measurements were carried out using a Dynamic Shear
Rheometer (DSR) to perform frequency sweeps at asphalt mixtures
service temperatures. The control PMBs and manufactured
bitumen-LR and bitumen-EBS blends were tested under the follow-
ing settings:

Oscillatory sweep frequency (0.1–10 Hz)

Strain control mode within the LVE region (1% strain), ampli-
tude sweep strain controlled tests were done to check the LVE
region

Multiple temperatures (0 °C–80 °C at 10 °C intervals)

Parallel plate geometry 8 mm diameter with 2 mm gap for low
temperatures (0 to 40 °C) and 25 mm diameter with 1 mm gap
for high temperatures (30 to 80 °C)
In these tests, binders’ rheological properties were measured in
terms of the norm of the complex (shear) modulus, |G*| (Pa), and
phase angle, d (⁰).
2.2.2. Phase II: Respond Surface methodology (RSM)
RSM was selected to study the combinations of LR and EBS to
have cost-effective binders and with desirable physical properties.
RSM is a useful tool to simultaneously study the effects of various
parameters and their interaction on specific responses using a col-
lection of statistical and mathematical techniques [17,13,26]. The
procedure for the design, modelling, analysis of variance (ANOVA),
and optimization of responses was carried out using Design Expert
9.0.6.2 software (Stat-Ease Inc.).
For this purpose, the dosage range of LR was established as 0–
50% and the dosage range of EBS was fixed as 0–6%. Within these
ranges, Design Expert 9.0.6.2 software suggested fourteen combi-
nations of LR and EBS as shown in Table 2. These combinations
were then tested to introduce the selected responses as inputs
before undertaking the RSM analysis and optimisation.
Three responses were selected to perform the optimisation: (1)
response at low temperature; (2) response at high temperature; (3)
cost.
2.2.2.1. Response at low temperatures. For pavement applications,
the SHRP fatigue parameter |G*| sin (d) at 1.59 Hz is widely used
to characterise and control the cracking resistance of binders. SHRP
has validated |G*| sin (d) as maximum as 5000 kPa to control the
fatigue resistance of flexible pavement [16]. Minimising |G*| sin
(d) would lower the dissipated energy per loading cycle; where,
minimum |G*| is favourable as softer binder will better dissipate
the work energy without developing large stresses, while binder
with lower d (more elastic) will regain to their original shape with
minimum dissipating energy. Therefore, this parameter was
selected as response to be minimised at 10 °C.
For roofing applications, the stiffness of bituminous materials at
low temperatures play a key role in controlling the thermal crack-
ing in roofing membranes. Too stiff binders develop high undesir-
able thermal stresses because the stress is directly proportional to
stiffness while more flexible binders can prevent stress build-up at
low temperatures. A loading frequency of 0.4 Hz has been sug-
gested to characterise the rheological properties of roofing binders;
at which a good agreement has been established between bitumen
rheological properties and bitumen empirical properties [2]. Thus,
the complex modulus |G*| at 0 °C and 0.4 Hz loading frequency was
selected to control the thermal cracking.
2.2.2.2. Response at high temperatures. In pavement engineering,
the SHRP rutting resistance parameter |G*|/sin(d) at 1.59 Hz can
give indication about the deformation resistance of binders at high
in-service temperatures where binders with higher |G*|/sin(d) are
preferable [16]. Therefore, this parameter was selected as response
to be maximised at 60 °C.
In the case of roofing, membranes manufacturing requires bitu-
mens with high melting point in order to produce a heavy coating
and to avoid permanent deformation under hot climatic condi-
tions. Thus, modified bitumens with higher softening point are
preferable for roofing membranes. Softening point was therefore
selected as response to be maximised. This test was carried out
in accordance with EN 1427 [39]. Softening point is defined as
the equi-viscous temperature measurement when the bitumen
softens enough and eventually deforms slowly to allow the steel
balls enveloped in bitumen to fall a distance of 25 mm into the bot-
tom plate.
2.2.2.3. Cost. The normalised cost of different blends was calculated
based on the relative cost of each component to the neat bitumen.
The cost of neat bitumen was considered as 1 unit, the liquid rub-
ber considered as 2.1 unit and the EBS as 3.45 unit. These unit
prices were computed based on their approximated cost in the
market.

Table 2
Matrix of experimental design factors and responses.

Dosage Responses (pavement) Responses (roofing)

Blend Liquid Rubber EBS |G*|sin(d) [MPa]@ |G*|/sin(d) [kPa]@ 60 °C, Unit |G*| [MPa]@ 0 °C, Softening point Unit
% % 10 °C,1.59 Hz 1.59 Hz Price 0.4 Hz [°C] Price
1 25 3 15.08 17.02 1.35 28.63 93.0 1.35
2 25 0 7.21 2.75 1.27 25.48 49.6 1.27
3 0 6 20.96 66.52 1.14 77.44 111.0 1.14
4 50 3 2.98 12.96 1.62 9.79 68.8 1.62
5 37.5 4.5 5.53 45.63 1.52 18.43 105.5 1.52
6 25 6 9.19 100.38 1.42 30.25 111.0 1.42
7 25 3 9.28 17.26 1.35 34.08 91.5 1.35
8 0 0 15.08 3.54 1.00 53.70 50.8 1.00
9 12.5 1.5 11.46 5.24 1.17 39.78 62.2 1.17
10 12.5 4.5 13.34 43.31 1.25 49.70 103.5 1.25
11 37.5 1.5 4.42 6.59 1.45 15.08 63.8 1.45
12 50 6 3.48 94.63 1.69 11.54 112.0 1.69
13 50 0 2.44 2.30 1.55 8.46 44.2 1.55
14 0 3 20.31 20.14 1.07 81.27 90.5 1.07
 A. Jiménez del Barco Carrión et al. / Construction and Building Materials 249 (2020) 118630 5

1.E+09

1.E+08

1.E+07

Comoplex Modulus |G*| (Pa)

1.E+06

1.E+05

1.E+04

1.E+03

1.E+02

1.E+01

1.E+00
0 10 20 30 40 50 60 70 80 90
Phase Angle ( )

Neat bitumen Blend 2 75/25/0 Blend 3 94/0/6 Blend 13 50/50/0

Blend 14 97/0/3 PMB (roofing) PMB (pavement)

Fig. 2. Black Diagram of the key binders.

1.E+09

1.E+08

1.E+07
Comoplex Modulus |G*| (Pa)

1.E+06

1.E+05

1.E+04

1.E+03

1.E+02

1.E+01

1.E+00
1.E-05 1.E-04 1.E-03 1.E-02 1.E-01 1.E+00 1.E+01 1.E+02 1.E+03 1.E+04 1.E+05 1.E+06
Reduced frequency (Hz)

Neat bitumen Blend 2 75/25/0 Blend 3 94/0/6 Blend 13 50/50/0

Blend 14 97/0/3 PMB (roofing) PMB (pavement)

Fig. 3. Master curves of the norm of the complex modulus at 30 °C reference temperature for the key binders.

Table 2 shows the measured responses for the fourteen combi- vidual desirability functions are different for different objective
nations suggested by Design Expert 9.0.6.2, where blends no. 2, 3, types which might be maximization, minimization or target. If
13 and 14 match those selected as first blends to study the influ- the objective type is maximum value, the desirability function is
ence of LR and EBS independently and will therefore be considered defined as [4]:
as key binders in the next sections. 8
>
< 0y <L

yL r
di ¼ TyL ð1Þ
2.2.3. Phase III: Optimisation >
:
TL

The desirability approach introduced by the Design Expert soft- 1y > T

ware were used to optimise simultaneously the different responses When the objective type is a minimum value, the individual
(Bezerra et al. 2008). The optimum situation of various responses is desirability (di ) is defined as:
identified after computing the overall desirability (D) of the con- 8
sidered responses. The individual desirability (di) is normalised >
< 1y <T

Uy r
into a dimensionless scale between 0 and 1, d = 0, for a completely di ¼ TyU ð2Þ
>
:
UT
undesirable response, and d = 1, for a fully desired response, above 0y > U
which further improvements would have no importance [4]. Indi-
6 A. Jiménez del Barco Carrión et al. / Construction and Building Materials 249 (2020) 118630
where y is the response that needs to be maximised or minimised to
a target value (T), L is the lower acceptable value and U is the upper
acceptable value to the response and r is the weight that attributes
levels of importance to the target value.
The following formula is then used to calculate the overall
desirability from the weighted geometric average of the individual
desirability (di):
1=m
D ¼ ðd1 d2    dm Þ
where m is the number of responses.
3. Results and discussion
3.1. Phase I: Individual influence of modifiers
Evaluating the LVE properties of binders under different loading
times and temperatures provides valuable information about the
predicted behaviour of binders under certain loading and environ-
mental condition. The stress–strain-time–temperature response of
the key and control binders was assessed by means of Dynamic
Mechanical Analysis (DMA) using a DSR as testing device. Black
diagrams, master curves of complex modulus |G*| and tan(d) at a
reference temperature of 30 °C using the Time-Temperature Super-
position Principle (TTSP) and William, Landel and Ferry (WLF)
equation were produced. The results are presented hereafter for
comparison.
3.1.1. Viscoelasticity
Black diagrams in Fig. 2 offer a convenient plot to show the rela-
tion between stiffness and viscoelasticity of materials without the
need to apply shift factors to the raw data as in the case of master
curves, being therefore considered as the fingerprint of the materi-
als [1]. The complexity and the different patterns of Black diagrams
for PMBs, LR and EBS modified bitumens demonstrate the sensitiv-
ity of phase angle measurements to the microstructural modifica-
tions and chemical structure that have been imparted by the
modifiers. In Fig. 2, Blends 2 and 13 represent the different levels
of modification of the neat bitumen with LR. It can be observed
that the addition of 25% LR does not significantly change the rheol-
ogy of the neat bitumen, while increasing up to 50% LR the material
16
14
12
10
TAN ( )
0
1.E-05 1.E-04 1.E-03 1.E-02
Neat bitumen Blend 2 75/25/0
Blend 14 97/0/3 PMB (roofing)
Fig. 4. Tan(d) master curve at 30 °C for the key binders.
experiments a noticeable increase of the elastic response at high
temperatures, reflected in the decrease of phase angle. On the
other hand, the modification of the neat bitumen with EBS (Blends
3 and 14) is remarkable from the lower level of EBS addition (3%).
EBS modification resulted in shifting the Black diagram curve at
high temperatures to higher complex modulus and decreased
phase angles. The comparison of the Black diagrams of LR and
EBS modification to PMBs reveals that these modifiers can provide
ð3Þ the same level of improved elastic response as in PMBs.
3.1.2. Stiffness
To further comparing the materials in terms of stiffness, their
complex modulus master curves are shown in Fig. 3. In this regard,
the master curves of PMBs represent the desirable LVE properties
that are sought for pavement and roofing applications, i.e. stiffer
and more elastic at high temperatures (low frequencies) to resist
permanent deformations; and softer and more flexible at low tem-
peratures (high frequencies) to cope with thermal cracking. These
particular features are reflected in the different shape of their master
curves which become flatter at low frequencies showing an increase
of their complex modulus with respect to the neat bitumen. Blends
3, 13 and 14 present the same tendency because of the presence of
modifiers. The complex modulus master curves have been fitted to
standard and generalised sigmoidal models [34].
Regarding LR, Blend 13, which has the highest content, has the
lowest complex modulus over most of temperatures and frequen-
cies. This reflects the ideal nature of LR to obtain modified binders
with enhanced physical properties to resist the low temperatures
thermal stresses and a noticeable recovery of elastic response in
terms of phase angle at high temperatures (Fig. 2) which would
help to resist plastic deformations. This is in line with the compo-
sition of the modifier that provides an overall decrease in rigidity
at intermediate and low temperatures, due to the enhanced elastic
behaviour conferred by the rubber and decrease in stiffness due to
the oils fraction. However, the resistance of materials to deforma-
tion at high temperatures would be significantly impaired.
On the other hand, EBS modification (Blends 3 and 14) resulted
in significant increase in the complex modulus of the neat bitumen
over the whole range of temperatures and frequencies. Conse-
quently, a proper combination of both Liquid Rubber and EBS, as
1.E-01 1.E+00 1.E+01 1.E+02 1.E+03 1.E+04 1.E+05 1.E+06
Reduced frequency (Hz)
Blend 3 94/0/6 Blend 13 50/50/0
PMB (pavement)
 A. Jiménez del Barco Carrión et al. / Construction and Building Materials 249 (2020) 118630 7

will be shown in the next sections, would produce bituminous 3.1.3. Temperature susceptibility
materials with enhanced physical properties that can adequately The loss tangent master curve is shown in Fig. 4 to examine the
resist the external stresses at both low and high temperatures in temperature susceptibility of materials. A plateau region or flatten-
terms of stiffness. ing of the tan(d) curves is desirable to have bituminous binders

Fig. 5. Effect of varying the amount of liquid rubber and EBS on the responses (pavement case).
8 A. Jiménez del Barco Carrión et al. / Construction and Building Materials 249 (2020) 118630

with enhanced temperature susceptibility [29,12]. A reduction in maintaining good flexibility to resist the cracking at intermediate
temperature susceptibility is important to produce a material that and low temperatures [12]. Fig. 4 confirms that the PMBs, Blends
is able to resist the deformation at high temperatures and also 3, 13 and 14 have the lowest temperature susceptibility as indi-

Fig. 6. Effect of varying the amount of liquid rubber and EBS on the responses (roofing case).
 A. Jiménez del Barco Carrión et al. / Construction and Building Materials 249 (2020) 118630 9

cated by their flat curves and comparable to the PMBs. On the other
hand, neat bitumen and Blend 2 have the largest change in tan(d)
over the range of frequencies and therefore the poorest tempera-
ture susceptibility. In the case of EBS, this fact is important in order
to understand how EBS is able to improve the temperature suscep-
tibility of the neat bitumen. In the case of LR, it can be noticed that
the dosage plays a great role, having that higher dosage produces a
less temperature-susceptible binder.
3.2. Phase II: Response surface methodology
In the RSM, first, the effects of LR and EBS dosages on the
defined responses were analysed independently. Next, prediction
laws of the responses as functions of LR and EBS dosages were
obtained by fitting the data to specific models and analysed.
3.2.1. Effects of LR and EBS
Considering the data in Phase 1, the effect of varying the
amount of LR and EBS on the main responses with 95% of statistical
confidence intervals are reported in Figs. 5 and 6. The figures
clearly demonstrate that increasing the LR content would signifi-
cantly decrease |G*| and |G*| sin(d) and increase the cost of binder.
The effect of LR on |G*|/sin(d) and softening point is neutral and no
significant change occurs with varying only the LR content. How-
ever, the effect of EBS is very significant on increasing the high
simultaneously evaluate the interaction effect of several factors
and suggest an appropriate model with respect to the responses.
The combining effects of using different dosages of LR and EBS
were, therefore, analysed using the RSM.
3.2.2. Prediction of responses by model fitting and analysis
The experimental results and the unit cost (calculated), shown
in Table 1, were used to develop mathematical models via RSM
to predict the different responses as functions of the LR and EBS
dosages. Statistical techniques, i.e. Analysis of variance (ANOVA),
F-tests, R-squared, lack of fit tests are utilised via RSM to find the
connections between factors and responses and then suggest the
appropriate model. In this study, the regression analysis shown
in Table 2 suggested that a linear model can be used for the soften-
ing point and unit cost, a second-order interaction model can be
used for |G*|sin(d) and quadratic models are the most appropriate
to predict |G*| and |G*|/sin(d).
A simple form of linear equation shown below is used to com-
pute the dependent responses [21,13]:
X
n
Y ¼ bo þ bi X i þ e ð4Þ
i¼1
The second-order interaction model is shown below:
X
n X
n1 X
n

in-service temperature properties (|G*|/sin(d) and Softening point). Y ¼ bo þ bi X i þ bij X i X j þ e ð5Þ

i¼1 i¼1 j¼iþ1
The unit price of binder increases with the addition of modifiers.
The unit price of adding 50% of LR could increase the binder cost The quadratic polynomial regression model is shown below:
by 50% while adding 6% of EBS could increase the binder cost by
15%. The analysis presented in Figs. 5 and 6 is based on changing X
n X
n X
n1 X
n
Y ¼ bo þ bi X i þ bii X 2i þ bij X i X j þ e ð6Þ
one-factor-at-a-time methodology. This analysis does not count i¼1 i¼1 i¼1 j¼iþ1
the interactions between parameters, and thus, the optimisation
process cannot be as efficient as the analysis when the influence where Y is the calculated response; X i andX j are the independent
of interacted parameters is taken into account. RSM is able to factors, LR and EBS dosages in this study; bo is the intercept; bi is

Table 3
The statistical parameters for the computed responses.

Response Item Sum of Squares DF Mean of Square F-value P-value Remark

|G*|[MPa]@ 0 °C, 0.4 Hz Model 7077.88 5 1415.58 68.19 < 0.0001 SD = 4.56Mean = 34.54R2 = 0.98R2predicted = 0.88
A-Liquid Rubber 6336.26 1 6336.26 305.21 < 0.0001
B-EBS 208.76 1 208.76 10.06 0.0132
AxB 117.04 1 117.04 5.64 0.0449
A2 409.42 1 409.42 19.72 0.0022
B2 63.24 1 63.24 3.05 0.1191
Residual 166.08 8 20.76
Lack of Fit 151.23 7 21.60 1.45 0.5656
|G*|.sin(d) [MPa]@ 10 °C, 1.59 Hz Model 451.58 3 150.53 30.90 < 0.0001 SD = 2.21
A-Liquid Rubber 430.18 1 430.18 88.30 < 0.0001 Mean = 10.05
B-EBS 15.44 1 15.44 3.17 0.1054 R2 = 0.90
AxB 5.96 1 5.96 1.22 0.2946 R2predicted = 0.86
Residual 48.72 10 4.87
Lack of Fit 31.90 9 3.54 0.21
|G*|/sin(d)[kPa]@ 60 °C,1.59 Hz Model 14520.57 4 3630.14 75.94 < 0.0001 SD = 6.91
A-Liquid rubber 66.16 1 66.16 1.38 0.2696 Mean = 31.30
B-EBS 12138.46 1 12138.46 253.92 < 0.0001 R2 = 0.97
AxB 205.88 1 205.88 4.31 0.0678 R2predicted = 0.87
B2 2110.08 1 2110.08 44.14 < 0.0001
Residual 430.23 9 47.80
Lack of Fit 430.20 8 53.78 1978.19 0.0174
Softening point [°C] Model 7709.29 2 3854.65 82.50 < 0.0001 SD = 6.84Mean = 82.67R2 = 0.94R2predicted = 0.90
A- Liquid Rubber 92.89 1 92.89 1.99 0.1862
B-EBS 7616.40 1 7616.40 163.01 < 0.0001
Residual 513.95 11 46.72
Lack of Fit 512.83 10 51.28 45.58 0.1148
Unit cost Model 0.57 2 0.28 8.4E + 5 < 0.0001 SD = 1.0Mean = 1.35R2 = 1.0R2predicted = 1.0
A- Liquid Rubber 0.53 1 0.53 1.6E + 6 < 0.0001
B-EBS 0.037 1 0.037 1.1E + 5 < 0.0001
Residual 3.689E-006 11 3.354E-007
Lack of Fit 3.689E-006 10 3.689E-007

DF, Degrees of Freedom; SD, Standard Deviation

10 A. Jiménez del Barco Carrión et al. / Construction and Building Materials 249 (2020) 118630
Fig. 7. Predicted vs. actual values of the selected responses (pavement), (a) |G*| sin(d) at 10℃ &1.59 Hz (b) |G*|/sin(d) at 60℃ & 1.59 Hz (c) unit cost.
Fig. 8. Predicted vs. actual values of the selected responses (roofing), (a) G* at 0℃ & 0.40 Hz (b) softening point ℃ (c) unit cost.
the linear coefficient (the gradient of the function), bii is the squared
coefficient, bij is the interaction coefficient and e is the random
error. Table 3 shows the statistical analysis of the suggested models
carried out by means of RSM. It can be seen that all the terms of
suggested models are statistically significant for 95% confidence
intervals from the fact that p-values are low compared to F-
values. The high regression coefficients shown in Table 3, R2 and
R2 predicted, indicate that the models can satisfactorily predict
the responses. The unit price of Bitumen/LR/EBS blends had already
been calculated based on linear relationship between the com-
pounds, therefore, it is expected to see a perfect regression analysis
for the actual and predicted values.
The final models calculated based on the regression coefficients
for the different responses are:
jG j0  C0:4 Hz ðMPaÞ ¼ 57:77  2:0  ðLR%Þ þ 6:89  ðEBS%Þ  0:07
 ðLR%Þ  ðEBS%Þ þ 0:02  ðLR%Þ2  0:05
 ðEBS%Þ2
jG jsinðdÞ10  C;1:59 Hz ðMPaÞ ¼ 15:22  0:27  ðLR%Þ þ 0:89  ðEBS%Þ
 0:016  ðLR%Þ  ðEBS%Þ
jG j=sinðdÞ60  C1:59 Hz ðkPaÞ ¼ 7:40  0:155  ðLR%Þ þ 6:90  ðEBS%Þ
 0:092  ðLR%Þ  ðEBS%Þ þ 3:08
 ðEBS%Þ2
 
Softening point C ¼ 53:33  0:145  ðLR%Þ þ 11  ðEBS%Þ
Unitcost ¼ 1:0 þ 0:011  ðLR%Þ þ 0:024  ðEBS%Þ
Figs. 7 and 8 show that there is adequate agreement between
the actual values of responses and the predicted ones. Thus, all
models can adequately be used to identify the optimal
situation.
The proposed models shown above can be plotted as a 2D (con-
tour) curve, or 3D surface using the Design Expert software as
shown in Figs. 9 and 10. The 2D and 3D contour plots, in Figs. 9
and 10, conveniently demonstrate the combination effect of both
LR and EBS on the responses in one plot. The method of steepest
ascent (or descent) can be used to find the direction towards max-
imization or minimization the responses [19]. The steepest ascents
(or descents) (the black arrows), shown in Figs. 9 and 10, are placed
perpendicular to the contours. It is relatively easy to identify the
optimum condition for each individual response. However, the
 A. Jiménez del Barco Carrión et al. / Construction and Building Materials 249 (2020) 118630 11

optimisation process becomes complicated when several
responses are considered. As can be seen the black arrows go in dif-
ferent direction for each response. The optimal value for each
response would, therefore, be localised in different conditions.
For example, minimization of the |G*|sin(d) is fulfilled by increas-
ing the LR and slightly decreasing the EBS while maximisation
the |G*|/sin (d) and softening point occurs by increasing the EBS
and slightly decreasing the LR. On the other hand, the cost of mod-
ified binder is minimised by reducing both LR and EBS. The desir-
ability function approach offered by the Design Expert software is a
very useful tool for dealing with multiple response optimisation.
This process is presented in the next section.

Fig. 9. 2D and 3D plots illustrated the effects of Liquid Rubber and EBS content on the main responses (pavement).
12 A. Jiménez del Barco Carrión et al. / Construction and Building Materials 249 (2020) 118630

Fig. 10. 2D and 3D plots illustrated the effects of Liquid Rubber and EBS content on the main responses (roofing).

3.3. Phase III: Optimisation For flexible pavement applications, the optimum LR and EBS
content was computed based on the requirements listed in Table 4.
The optimisation process for flexible pavement applications and The limit constrains for the responses were selected to be within
roofing applications was conducted separately. 10% of PMB properties that are used in pavement.
 A. Jiménez del Barco Carrión et al. / Construction and Building Materials 249 (2020) 118630 13

Table 4
Optimisation criteria used in the case of pavement application.

Factors or responses Target Constraints PMB

Lower limit Upper limit
A:Liquid Rubber in range 0% 50% ——
B:EBS in range 0% 6% ——
|G*| sin(d) @ 10 °C&1.59 Hz [MPa] minimise 6.85 8.40 7.6
|G*| / sin (d) @ 60 °C&1.59 Hz [kPa] maximise 4.50 5.50 5
Unit price minimise 1.00 1.50 1.5 to 2

Fig. 11. Identify the optimal combination of liquid rubber and EBS that give the
Fig. 12. Identify the optimal combination of liquid rubber and EBS that give the
best desirability for pavement application.
best desirability for roofing application.

Figs. 11 and 12 show how the desirability functions and the val-
ues of responses change with the amount of LR and EBS. The desir-
A: Liquid Rubber = 33.88%
able responses of |G*| and |G*|sin(d) were set as being a minimum
B: EBS = 1.83%
to attain a modified binder with improved flexibility behaviour at
The corresponding responses are:
intermediate or low temperatures. And, the desirable response of |
|G*|.sin(d) @ 10 ⁰C &1.59 Hz (MPa) = 6.85
G*|/sin(d) and softening point were set as being a maximum to
|G*|/sin(d) @ 60 ⁰C &1.59 Hz (kPa) = 5.5
have binders with enhanced rutting resistance at high tempera-
Cost (Unit) = 1.41
tures. Finally, the Unit price was set as being minimum.
The amount of LR and EBS proposed by the software to simulta- For roofing applications, the optimum LR and EBS content was
neously satisfy all responses for pavement applications are: computed based on the requirements listed in Table 5.
14 A. Jiménez del Barco Carrión et al. / Construction and Building Materials 249 (2020) 118630
Table 5
Optimisation criteria used in the case of roofing application.
Factors or responses Target
A:Liquid Rubber in range
B:EBS in range
|G*| @ 0 °C &0.40 Hz [MPa] minimise
Softening point [°C] maximise
Cost [unit] minimise
The amount of LR and EBS proposed by the software to simulta-
neously satisfy all responses for roofing applications are:

A: Liquid Rubber = 38%

B: EBS = 4%

The corresponded responses are:

|G*|@ 0 ⁰C&0.4 Hz (MPa) = 18.78

Softening Point (C) = 92

Cost (Unit) = 1.51
In this regard, it can be seen that the desirability functions are
suitable to identify the amount of modifiers that lead to the opti-
mal compromises.
4. Conclusions
This paper develops and optimises the use of recycled tyre rub-
ber (RTR) in high content as bitumen modifier for pavement engi-
neering and roofing applications. To do this, the RTR was
incorporated in form of Liquid Rubber (LR), an innovative delivery
method ensuring storage stability of the recycled polymer, in com-
bination with the wax EBS. Firstly, key blends of bitumen and LR or
EBS were rheologically characterised to obtain their linear visco-
elastic properties. Next, for the purpose of optimising the design
of the blends with more than two components, the Response Sur-
face Methodology was applied by using high temperature, low
temperature and cost of PMBs as design targets.
In the light of the results presented, the following conclusions
can be drawn:

The proposed bitumen modification methodology and design
procedure allows designing bituminous blend with mechanical
properties and cost comparable to PMBs (±10%) currently used
for asphalt mixtures and roofing membranes. These blends are
engineered to totally replacing SBS in favour of a combination
of a recycled polymer (RTR) and a wax (EBS).

The two modifiers both increase elasticity of bitumen and
seems to balance each other in terms of stiffness. In fact, the oils
of the LR reduces the stiffness of the base bitumen while the EBS
has shown to effectively increasing the stiffness and elasticity of
the blends allowing therefore to cope with drawbacks of high LR
contents to be used.

The RSM is a powerful tool to engineering new bituminous
blends by predicting the response of the materials on the basis
of experimental plans crafted with a statistical approach. In this
regard, for the final blends, linear functions were found to cor-
relate the softening point and cost to LR and EBS dosages, while
a second-order interaction model was found for
jG jsinðdÞ10  C1:59 Hz and a quadratic polynomial functions were
applied to jG j0  C0:4 Hz andjG j=sinðdÞ60  C1:59 Hz .

The final optimal composition of blends includes LR contents in
the range of 30–40% by weight of base bitumen. These contents
imply the use of 15–20% of RTR (due to the LR composition of
50% RTR + 50% heavy oils) while further reducing the need for
virgin bitumens in terms of total modification percentages for
pavement engineering and roofing applications.
Constraints PMB
Lower limit Upper limit
0% 50% ——
0% 6% ——
16 20 17
90 110 102
1 1.52 1.5 to 2
The proposed optimal composition of bitumen, LR and EBS
blends for pavement engineering and roofing applications are
being validated in the laboratory in terms of performance-related
properties and ageing. Further research will look at the perfor-
mance of asphalt mixtures and roofing membranes manufactured
with the designed binder. Other research should look also a com-
paring the environmental impact of the proposed solutions.
5. Data availability
The raw/processed data required to reproduce these findings
cannot be shared at this time as the data also forms part of an
ongoing study.
CRediT authorship contribution statement
Ana Jiménez del Barco Carrión: Investigation, Writing - review
& editing. Ayad Subhy: Formal analysis, Visualization, Writing -
review & editing. Maria Angeles Izquierdo Rodriguez: Conceptu-
alization, Investigation, Writing - review & editing. Davide Lo
Presti: Conceptualization, Methodology, Supervision, Funding
acquisition, Writing - review & editing.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
Acknowledgements
This work is part of a research project sponsored by a KTP Pro-
gramme (Knowledge Transfer Partnership No. KTP9265). The
authors gratefully acknowledge its financial support. Finally, this
work was partially supported by the Italian Ministry of University
and Research (MIUR dm n.372 08/05/18).
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