Construction and Building Materials 106 (2016) 290–295

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Construction and Building Materials

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

Rheological studies of asphalt modified with elastomeric polymer

Dennyele Alves Gama a,b,⇑, José Manoel Rosa Júnior c, Tomas Jeferson Alves de Melo d,
John Kennedy Guedes Rodrigues e
a
Science and Engineering of Materials, Federal University of Campina Grande – UFCG, PB, Brazil
b
Laboratory of Pavements Engineering, UFCG, Brazil
c
Civil Engineering and Environmental, Federal University of Campina Grande – UFCG, PB, Brazil
d
Materials Science and Engineering, Federal University of Campina Grande – UFCG, PB, Brazil
e
Civil Engineering, Federal University of Campina Grande – UFCG, PB, Brazil

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

Article history: Reactive polymers, consisting of glycidyl methacrylate, produce a chemical reaction between the polymer
Received 7 July 2015 and the asphalt binder that can be beneficial for asphalt application in hot climates. Elastomeric-modified-
Received in revised form 16 December 2015 bitumen mixes were developed using elastomeric polymer (EMA-GMA), high density polyethylene (HDPE)
Accepted 21 December 2015
and polyphosphoric acid (PPA 116%). Physical and rheological properties of modified bitumen, complex
modulus (|G⁄|), phase angle (d), and MSCR test were analyzed. Test results of penetration, softening point
and elastic recovery showed an increase of elastic behavior in modified asphalts and produced material
Keywords:
properties suitable for application in highway construction. Based on rheological test results, it was
Polymers
Functionalization
observed that the addition of polymer can increase the range of temperature, in asphalt, to resist permanent
Reactive polymers deformation. MSCR test results characterize the modified asphalt as an elastomeric with good performance
Modified asphalt at intermediate temperatures.
Elastomeric Ó 2015 Elsevier Ltd. All rights reserved.
Rheology

1. Introduction
An asphalt-layer’s rheological properties can be altered when
subjected to ambient-temperature changes, resulting in a
reduction of viscosity, making the asphalt more susceptible to
permanent deformation. The asphalt can also be affected by other
factors such as vehicle type and high-traffic volume—one of the
main factors that determines the life of the pavement—which
ultimately limit durability. However, it is possible to reduce
permanent deformation in asphalt by increasing the stiffness of
the binder through modification of its properties with the use of
polymeric materials [1].
Polymers used for asphalt modification can be grouped into
three main categories: thermoplastic elastomers, plastomers, and
reactive polymers. Every polymer used in modification creates a
specific effect and alters properties within an asphalt mixture.
Thermoplastic elastomers used to achieve good elastic properties
in a modified binder, while plastomers and reactive polymers are
⇑ Corresponding author at: Science and Engineering of Materials, Federal
University of Campina Grande – UFCG, PB, Brazil.
E-mail addresses: dennyele@hotmail.com (D.A. Gama), jmarj10@yahoo.com.br
(J.M. Rosa Júnior), tomas@dema.ufcg.edu.br (T.J.A. de Melo), profkennedy@hotmail.
com (J.K.G. Rodrigues).
added to improve rigidity and reduce deformation under load [2].
Careful measures must be taken when using polymers in asphalt
mixtures. It is important to consider the possibility of phase sepa-
ration due to incompatibility of polymers used, separation can
occur when materials are stored at high temperatures.
The functionalization of polymers has shown a promising alter-
native to reduce disadvantages presented by some types of poly-
mers in modifying asphalt binders. In bitumen polymer
modification, functionalization relates to the chemical addition of
specific polymers to obtain specific characteristics within modified
asphalt. Modified-characteristics such as: good storage stability,
excellent ageing resistance, strong adhesion with aggregates, high
stiffness at high temperatures and good cracking resistance at low
temperatures are desired in asphalt mixes used in hot climates.
Functionalization is a tool that can be used to increase the quality
level of polymer-modified bitumens which will ultimately affect
durability and serviceability in the future [3].
Various mixes of asphalt modified with polymer (PMB) may be
obtained through functionalization; however, current investiga-
tion is mainly focused on improving compatibility of polymer
modifiers with bitumen. Based on test results, reactive polymers
are new polymer modifiers that, through functionalization, can
be used for the development of new asphalt-modified mixes.
Reactive polymers used in bitumen modification are polymers

http://dx.doi.org/10.1016/j.conbuildmat.2015.12.142
0950-0618/Ó 2015 Elsevier Ltd. All rights reserved.
 D.A. Gama et al. / Construction and Building Materials 106 (2016) 290–295
believed to chemically react (rather than physically mix or inter-
act) with some components of bitumen.
Reactive polymers are not commonly used as modifiers in
asphalt; however previous work has shown that glycidyl-
methacrylate-based polymers have shown to chemically react with
asphalt binder [4]. This reaction results in the formation of an
asphalt copolymer, which causes changes in the properties of the
asphalt binder—specifically those regarding temperature sensibil-
ity. In a modified asphalt mixture, better resistance to variation
in temperature can result in a mixture which is more resistant to
permanent deformation. Additionally, the use of reactive polymers
has not shown phase separation problems observed with in mixes
using other polymers [3].
Glycidyl-methacrylate polymers (GMA) have shown to improve
the storage stability and other binder properties when used as
reactive polymers in asphalt binders [4,5–8].
In addition to the previously mentioned polymers, polyphos-
phoric acid (PPA), has already been used as a binder modifier.
The polyphosphoric acid can be used together with other modi-
fiers, like polymers, resulting in a chemical change of the binder
which can result in improvement of modified asphalt. [9]. PPA
has the following effects on an asphalt when used in modification:
As a catalytic, it improves the softening point without changing
stiffness; as a direct additive, it increases high-temperature resis-
tivity—due to the reaction of asphaltenes and the acid—and as an
accelerator, it can be used to lower amount of polymer needed in
a modified mixture [10,11].
An effective way to understand the internal structure of a
polymer-modified asphalt binder is through rheological study.
Rheological tests measure a wide range of material properties that
can be analyzed to determine a binder’s fundamental characteris-
tics. The development of property-specific polymer blends is diffi-
cult since modification causes a change in both rheological and
mechanical properties of a binder [12].
Rheological properties, gathered from rheological tests, are per-
formed under linear viscoelastic conditions (LVE). At linear vis-
coelastic condition, properties are measured where the
relationship between stresses and strains are influenced only by
temperature and loading time and not by magnitude. The LVE rheo-
logical properties of bitumen are normally presented in the form of
both the complex modulus (|G⁄|) and phase angle (d) master curves.
The |G⁄| is defined as the ratio of maximum (shear) stress to maxi-
mum strain when subjected to shear loading and d is the phase dif-
ference between stress and strain in harmonic oscillation. The
laboratory equipment to determine these rheological properties is
the dynamic shear rheometer (DSR). The frequency sweep configu-
ration is normally adopted to establish the response of bitumen to
different loading frequencies, in terms of |G⁄| and d. The mechanical
response of asphalt composites is frequently modeled by computa-
tional methods [13].
The parameter G⁄ can be related to resistance to permanent
deformation when an asphalt road is subjected to shear stress. The
phase angle (d) is a function of a viscoelastic response of the material.
When a material is a pure elastic, the d is zero degrees, and the vis-
coelastic response to deformation is immediate—however, when d.
90° the material behaves like a purely viscous material. The tan d
provides an indication of balance of viscoelastic behavior. High
values of G⁄ represent an increase in stiffness of material, while
low values of d represent improvement in elastic response [14,15].
Classification made through Superior Performance Pavement
(SUPERPAVE,SHRP) emphasize the parameter G⁄/send, as a better
criterion to determine the maximum use temperature for the binder
to ensure good performance.
This paper presents an analysis of rheological properties of bin-
der modified with polymers. Binders were modified using reactive
polymer (RET), polyphosphoric acid (PPA 116%) and high density
291
polyethylene (HDPE). The properties analyzed through laboratory
tests are: complex modulus (G⁄), temperature sweep, performance
grade (PG) and multiple stress creep and recovery (MSCR).
Observations made on softening point, elastic recovery, penetra-
tion and rheological measurements are also included.
2. Experiment and methods
2.1. Materials
Asphalt cement, with classification PG 64-XX, from Replan
refinery was used to produce laboratory modified asphalt samples.
The following polymers were used for modification: Ethylene–Me
thyl-Acrylate–Glycidyl-Methacrylate commercially named by
Polimul S74Ò, High-Density Polyethylene, Polimul SX500Ò, and
Polyphosphoric Acid PPA 116% (manufactured by PRANA Petro-
chemical Company S.A.).
2.2. Methods
Five different asphalt samples were tested. The samples were
comprised of one pure asphalt (PG 67-XX, unmodified), and four
binder samples modified with 1.8%wt of S74 plus SX500 (amounts
of 0.0, 0.1, 0.3 and 0.5 wt%)—each containing 0.15%wt of PPA as cat-
alyst. The modified binders were prepared in a mechanical mixer
model Fisatom 72 mixed at 500 rpm at a temperature of 170 °C.
Modified samples were prepared using 1.8 wt% of Polimul S74
mixed for a period of 1 h, Polimul SX500 was then added (0.0,
0.1, 0.3 or 0.5%wt) and mixed for 30 min and finally, PPA 116%
was added and mixed for 30 min. After completion on mixing,
samples were oven-cured for a period of 12 h.
Samples were labeled PA (Pure Asphalt), S74 (Polimul S74
added) and S74 SX (Polimul SX500 added follow by amount %wt).
2.3. Test methods
2.3.1. Softening point
Softening Point was performed according to ASTMD36. A steel
ball on a ring filled with bitumen sample is cooled in a water bath
oven with 5 °C ice water. After 15 min in water bath, the sample is
heated with a heat-up rate of 5 °C/min. The temperature is
recorded once the steel ball falls 25.4 mm. This temperature is
recorded as the softening point of the sample.
2.3.2. Elastic recover
Elastic Recover, by ductilometer, was performed according to
ASTM D6084. Specimens are pulled a 20 cm distance at a 5 cm/
min rate and at a constant 25 °C temperature. Elastic recovery is
the percentage of return of sample to original condition after
elongation.
2.3.3. Penetration
Penetration is a depth measurement. The test is performed by
vertically penetrating a needle using a 100 g weight, during a 5 s
interval at a constant 25 °C temperature. Penetration is related to
stiffness of the binder at ambient temperature and serves as a clas-
sification parameter for binders.
2.3.4. Rheological measurements
These oscillatory tests are performed using dynamic shear
rheometers (DSR), which apply oscillating shear stresses and
strains to samples of bitumen inserted between parallel plates at
different loading frequencies and temperatures. Measurements of
the complex shear modulus (G⁄), storage modulus (G0 ) and shear
292 D.A. Gama et al. / Construction and Building Materials 106 (2016) 290–295
loss modulus (G00 ) were carried out using a DHR-1 Rheometer man-
ufactured by TA Instruments.
The parameter tand = G00 /G0 is used as a measure of the relative
elasticity of the binders studied. Using the relationship previously
mentioned, the lower the value of tand, the more elastic the
system.
The MSCR evaluates the non-recoverable compliance, the per-
centage of recovery and the sensitivity of asphalt binder to varia-
tions in voltage level [16]. The test is performed according to
ASTM D-7405-08 which subjects a sample of asphalt binder in
PG temperature to a controlled tension for a period of one second.
After tension is induced, the sample is removed and allowed to rest
for a period of nine seconds. Two voltage levels are used to simu-
late low and heavy traffic conditions, 100 Pa applied to the first ten
cycles and a second 3200 Pa, applied for the next ten cycles [17].
At the end of each cycle of fluency and recovery the following
information is logged:
e0 = er = fluence at the beginning of each cycle at time 0 s;
ec = fluence at the end of each cycle time of 1 s;
et = creep recovery at the end of each cycle time of 10 s.
With the above information, the non-recoverable complacency
Jnr (r, N); the stress r = r = 100 Pa or 3200 Pa; and, the% recovery
percentage R (r, N) for each cycle creep and recovery (where N is
the number of cycles 1 6 N 6 10) are calculated using Eqs. (1)
and (2). The value of Jnr (r, N) and %R (r, N) is the average of the
values obtained for the 10 cycles performed during the test.
ðer  e0 Þ
J nr ðr; NÞ ¼
r
fðer  e0 Þ  ðer  e0 Þg  100
%Rðr; NÞ ¼
ðeC  e0 Þ
Repeated creep tests have been used to evaluate the modified bin-
der with positive results, demonstrating the sensitivity of this
method to identify the effect of polymer and asphalt additives in
the performance of asphalt binder [18].
3. Results and discussion
3.1. Softening point
Softening point is used to evaluate the high-temperature per-
formance of modified asphalt. According to Fig. 1, the softening
point of modified bitumen increases as polymer content increases.
Based on results, there is a considerable increase in softening point
temperature between the pure asphalt and the S74 modified
asphalt samples. In addition, there is further increase in softening
Fig. 1. Softening point of pure and modified binders.
point due to addition of SX500 polymer into the mixtures. When
compared to pure asphalt (PA), addition of polymer created an
increase in softening point of 17.5 °C in the S74 modified asphalt
and of 21.6 °C, 28.5 °C and 33.5 °C—respectively—in the SX500
modified samples.
Test results show that stiffness of modified asphalt improves
with the addition of polymers, especially when SX500 is added.
SX500 is a polyethylene of high-density, classified as a thermoplas-
tic, which improves material properties of modified asphalts to
better perform at high temperatures.
3.2. Elastic recover
The elastic recover (ER) at 25 °C is a measurement which deter-
mines the degree to which a substance recovers its original shape
following application and release of stress. A high degree of elastic
recovery is desirable in pavement to avoid permanent deforma-
tion. Table 1 shows the values of ER (%) of bitumen before and after
addition of polymers. Elastomeric polymers, used in mix S74, con-
tribute to improvement of elastic properties thus potentially
reducing permanent deformation of asphalt binders. The SX500
modified samples, show an increase in elastic properties. Increase
in elasticity of SX500 samples was achieved through use of small
amounts of polymer. Sample S74 SX 0.3 exhibited the largest RE
value observed with an 87.4% recovery rate.
3.3. Penetration
Penetration is an experimental parameter to describe the
ð1Þ temperature-susceptibility of bitumen. According to Table 1,
shown below, the addition of polymer resulted in a reduction of
penetration. Test results show that addition of polymer results in
ð2Þ improvement of modified asphalt hardness which can result in
improvement of permanent deformation. All penetration values
measured fall within the limits set by Brazilian classification for
elastomeric binders 60/85-E—minimum penetration of 40 dmm.
3.4. Performance grade (rutting resistance at high temperature)
The SUPERPAVE specification uses the parameter G⁄/send to
control stiffness of asphalt binder at high temperatures. The
parameter also provides the maximum temperature to maintain
resistance and elasticity, as well as, the maximum temperature
to preserve adequate performance.
Table 2 shows the maximum temperature of PG for pure and aged
binders tested. The PG temperature presented is the maximum tem-
perature at which the pure binder shows G⁄/send P 1 kPa and the
aged binder G⁄/send P 2.2 kPa.
The PG temperatures presented are based only on maximum
temperature, to represent binders being placed in hot climates.
Analysis of data showed that addition of modifiers increased the
maximum temperatures at which the pure binder shows
G⁄/send P 1 kPa and the aged binder G⁄/send P 2.2 kPa—also evi-
denced by the high PG recorded. It is worth mentioning that at low
temperatures the modified samples show different values for
G⁄/send parameter; however, with addition of modifiers G⁄/send
Table 1
Elastic recover and penetration results.
Elastic recovery (%) Penetration (dmm)
PA 10.0 64.08
S74 83.0 49.50
S74 SX 0.1 85.8 45.30
S74 SX 0.3 87.4 44.40
S74 SX 0.5 86.0 43.45
 D.A. Gama et al. / Construction and Building Materials 106 (2016) 290–295 293

Table 2
PG of binders.

Maximum temperature (°C) Maximum temperature (°C) PG

G⁄/send P 1 kPa pure binder G⁄/send P 2.2 kPa ager binder
PA 64 64 64
S74 82 70 70
S74 SX 0.1 82 76 76
S74 SX 0.3 82 76 76
S74 SX 0.5 82 76 76

follows a similar trend as those presented above. As a result, G⁄/send

values measured in this study conclusively show that addition of
modifiers increased resistance to permanent deformation of
asphalts studied.

3.5. Complex modulus (G*) and phase angle (d) in temperature stiffness

The complex modulus is related to stiffness of asphalt binder

and represents resistance to permanent deformation. Fig. 2 shows
the Complex Modulus curves with temperature ranging between
46 and 82 °C for pure binder and modified binders used in this
study.
It can be observed that there is a considerable increase in
G⁄/send for the S74 binder, due to the change of chemical structure
of the binder as a result of modification. For samples: S74, SX 0.1, Fig. 3. Range of tand with temperature in modified binders.
S74 SX 0.3 and S74 SX 0.5, the addition of Polimul SX500 resulted
in changes of complex modulus. The highest G⁄ value is recorded in
the S74 SX 0.5 sample, at low temperatures, which included 0.5 wt phenomenon can also be observed on Table 1 results, where mix
% of SX500 for modification. Furthermore, at high temperatures all SX 0.3 had a better elastic recovery rate than mix SX 0.5
modified samples show the same level of quality, in terms of
stiffness.
3.6. Multiple stress creep recovery (MSCR) test
In terms of elasticity, tand is used to characterize improvements
in elastic properties (G0 ) of modified binders. Improvement in elas-
Fig. 4 shows the values of percentage of recovery in two levels
tic properties is indicated through reduction of the tand parameter.
of stress for the pure and modified binder. In general terms, the
The results from this study were used to create a comparative anal-
MSCR recovery percentage (%Rec) measurement can identify and
ysis of elasticity between the pure and modified binders. Test
quantify the effect of the polymer in the binder. It can be observed
results show that addition of modifiers results in a significant
that the pure binder has almost zero%Rec at high stress, and about
reduction of tand values, suggesting an improvement of elastic
15.75%Rec at low stress. The addition of polymers improves the %
response of studied binders.
Rec of modified asphalt at the both levels of stress, 100 Pa and
Fig. 3 depicts results for modified binders analyzed. Results
3200 Pa. Improvement of %Rec results in improvement of a modi-
show a reduction of tand values with an increase in polymer con-
fied binder to maintain elastic characteristics at high-levels of
tent in binder mix. In addition, test results show that increased
traffic.
addition of SX500 results in further reduction of tand values mea-
Test results show that at 100 Pa, the %Rec ranges from 15.7%
sured—showcasing advantages of using this polymer to improve
Rec—for pure binder—to 95.8%Rec—for SX500 modified binder. At
elastic properties. From the data shown, mix SX 0.5 appears to have
3200 Pa stress, the percentage of recovery ranges from 2.4%Rec—
higher tand values than mix SX 0.3 after a temperature of 50 °C is
for pure binder—to 91.5%Rec—for S74 SX 0.5 composition.
reached. The reason attributed to this was a possible saturation
Recovery percentage values for pure asphalt differ greatly when
point of polymer related to this property at this temperature. This
tested at 100 Pa—low-traffic—and 3200 Pa—heavy-traffic. Large
differences in recovery percentage measured, for pure asphalt,

Fig. 2. Range of complex modulus with temperature in pure and modified binders. Fig. 4. Binder percentage of recovery before and after addition of polymers.
294 D.A. Gama et al. / Construction and Building Materials 106 (2016) 290–295
Fig. 5. Polymer modification validation curve for 3200 Pa stress-level.
Fig. 6. Percentage of non-recovery compliance to 3200 Pa.
between the two stress-levels tested result in poor pavement per-
formance. Addition of polymers into the binder mix resulted in an
overall increase of recovery percentage for both low and high traf-
fic scenarios. Furthermore, data shows a small difference in recov-
ery percentage drop between low and high traffic levels when
polymers are used. This is an indication that polymer modification
can be used to improve performance of low and high traffic
pavements.
Using the above mentioned data, a relation between %Recovery
and Jnr—at 3200 Pa—can be performed to validate use of polymer
modification. The curve stops at Jnr = 0.5 kPa1 and 0.1 kPa1. Jnr
values greater than 0.5 kPa1 are not required to have any mini-
mum %Rec value. Jnr values less than 0.10 kPa1 are required to
have a minimum %Rec value of 55%.
Percent recovery and non-recoverable compliance can be used
to assess appropriate level of polymer for use in modified asphalt.
The solid line shown on Fig. 5 presents the empirical reference
curve for proper polymer content in bitumen. Results located
above the reference curve indicate use of proper amount of poly-
mer in mixture. Pure asphalt and S74 modified results are located
below the reference curve—showing incorrect use and insufficient
dosage of polymer. Asphalts modified with SX500 results, at every
concentration, are located above the reference curve—showing
appropriate levels of percent recovery and thus be classified as
modified asphalts. Values of Jnr 3200 Pa for S74 SX500 modified
asphalt are close to zero. Jnr is a relation between unrecovered
shear strain and applied shear stress. From test results, it can be
concluded that these modifiers have slow unrecovered strain for
3200 Pa.
Fig. 6 illustrates the percentage of Non-Recovery compliance
(Jnr, diff%).
To minimize concerns that some asphalt binders may be overly
sensitive to changes in shear stress, AASHTO MP19 maintains a
requirement that the difference in Jnr values between 100 Pa and
3200 kPa shear stress should not exceed a ratio of 75%. Therefore,
S74 SX0.5 exceeds this criterion with a Jnr difference of 109.5%.
Analyzing the results of Jnr difference of the studied samples, only
the value for S74 SX0.5 sample exceeded AASHTO MP19 limits. This
highlights the high sensitivity of this sample to voltage level change.
From these observations it can be concluded that use of SX500 must
be limited to 0.3%wt to maintain good properties of modified
asphalt.
4. Conclusions
The related results confirmed the efficiency of addition of poly-
mers into asphalt binder. Polymer addition provides improvements
of physical and rheological properties of modified binder when
compared to pure, unmodified binder. The test conducted in this
study measured elastic recovery, softening point and rheological
properties. The empirical tests were performed at 25 °C, and
showed an increase of percentage of elastic recovery of modified
binder when Polimul SX500 contents were added into asphalt.
The softening point increased with polymer addition, showing
improvement of permanent deformation.
Rheological tests further showcased the positive effects of poly-
mers when mixed into asphalt binders. Polymer addition resulted
in an increase of PG, thus improving behavior of asphalt binder to a
higher range of working temperatures. Increase in complex modu-
lus, due to polymer addition, resulted in improvement of perma-
nent deformation of modified binders. Elastic response was
measured at different levels of stress, results show sample S74
SX0.3 to have optimum behavior—showing high levels of recovery
at low and high stress.
In conclusion, use of Polimul S74 showed improvement on elastic
behavior of asphalt. Addition of Polimul SX500 provided an increase
in both stiffness and elastic response. Using these polymers together
can result in a modified asphalt mixture with high-working-
performance at high and intermediate temperatures.
Acknowledgment
To PRANA Petrochemical to provide the materials for this
research.
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