Materials and Design 68 (2015) 8896

Contents lists available at ScienceDirect

Materials and Design

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

Stiffness modulus of Polyethylene Terephthalate modied asphalt

mixture: A statistical analysis of the laboratory testing results
Taher Baghaee Moghaddam , Mehrtash Soltani, Mohamed Rehan Karim
Center for Transportation Research, Department of Civil Engineering, Faculty of Engineering, University of Malaya, 50603 Kuala Lumpur, Malaysia

a r t i c l e

i n f o

Article history:
Received 14 September 2014
Accepted 25 November 2014
Available online 10 December 2014
Keywords:
Asphalt mixture
Mixture stiffness
Waste Polyethylene Terephthalate
Environmental temperature
Applied stress
Response Surface Methodology

a b s t r a c t
Stiffness of asphalt mixture is a fundamental design parameter of exible pavement. According to literature, stiffness value is very susceptible to environmental and loading conditions. In this paper, effects of
applied stress and temperature on the stiffness modulus of unmodied and Polyethylene Terephthalate
(PET) modied asphalt mixtures were evaluated using Response Surface Methodology (RSM). A quadratic
model was successfully tted to the experimental data. Based on the results achieved in this study, the
temperature variation had the highest impact on the mixtures stiffness. Besides, PET content and amount
of stress showed to have almost the same effect on the stiffness of mixtures. The optimal amount of PET
was found to be 0.41% by weight of aggregate particles to reach the highest stiffness value.
2014 Elsevier Ltd. All rights reserved.

1. Introduction
Stiffness of asphalt mixture is a fundamental design parameter
of exible pavement. It was found that there is a correlation
between stiffness and other mixture properties such as rutting
and fatigue, and thus it can be used as a criterion to evaluate
Asphalt Concrete (AC) mixture performance [1]. As it is mentioned
by Strategic Highway Research Program (SHRP) the stiffness value
of AC mixture is very susceptible to environmental temperature
and loading conditions [2].
Stone Mastic Asphalt (SMA) is gap-graded AC mixture which
has been developed in Germany in 1916s. SMA consists of more
course aggregate particles, mineral ller and asphalt binder. Due
to inherited structure of SMA, it provides better permanent deformation (rutting) performance and durability compared to conventional dense-graded mixture [3,4]. Draindown is a common
problem in SMA mixture because it contains higher amount of
asphalt binder. Hence, to prevent from draindown in SMA mixture
stabilizer additives, bers and polymers are used. Using polymer in
SMA mixture is very common. Utilizing polymer in SMA mixture
prevents not only from the binder draindown but also it can
enhance mixture performance [5,6]. In many cases, using polymers
causes higher construction cost due to high cost of polymers. To

Corresponding author. Tel.: +60 108927064; fax: +60 379552182.

E-mail addresses: p.baghaee@gmail.com, payam_baghaei@siswa.um.edu.my
(T. Baghaee Moghaddam).
http://dx.doi.org/10.1016/j.matdes.2014.11.044
0261-3069/ 2014 Elsevier Ltd. All rights reserved.

overcome this disadvantage, many studies investigated using

waste polymers in asphalt mixtures [68].
One of the important industrial plastic materials is Polyethylene
Terephthalate (PET). PET is a semi-crystalline thermo plastic polymer material which is used in beverage and food industries for
years. Nowadays, a large amount of waste PET is produced in the
world and it is going to cause a serious environmental challenge
due to non-biodegradability of PET [9]. Hence, some studies have
been previously performed to evaluate the effects of using postconsumer PET as secondary materials in road pavement in order
to nd solutions to tackle with this potential environmental hazard
and, moreover, to decrease construction cost imposed by application of polymers in asphalt mixture [6,1012].
Statistical analysis is a precise and popular way to explore and
present interactions between parameters affecting one phenomenon. Statistical analysis in pavement engineering has prominent
utilization because it helps road engineers and designers to have
better perspective about the pavement performance parameters.
In this case, factorial Design of Experiments (DOE) which through
the use of techniques such as Response Surface Methodology
(RSM) simultaneously consider several factors at different levels,
and give a suitable model for the relationship between the various
factors and the response came into popularity [1315].
Aim of this study was examining the AC mixture stiffness at elevated temperatures and stress levels for the unmodied and PET
modied mixtures following by nding interactions between these
fundamental factors using RSM based on Central Composite Design
(CCD).

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T. Baghaee Moghaddam et al. / Materials and Design 68 (2015) 8896

2. Materials and methods

Asphalt mixtures were fabricated using 80100 asphalt penetration grade. Granite-rich aggregate particles were used for this
investigation. 9% of ller was utilized. The aggregate particle size
distribution is shown in Fig. 1. In order to have better understanding about the materials characteristics several tests were performed on asphalt cement and aggregate particles and the results
are listed in Table 1.
PET akes have been used for this study which were obtained
from waste PET bottles. For using PET akes in asphalt mixture,
the PET bottles were cut to small parts and by using crushing
machine these small parts were crushed. Thereafter, the crushed
PET particles were sieved and the particles which were smaller
than 2.36 mm in size were used for this investigation.
2.1. Mixture fabrication
In order to fabricate SMA mixture, 1100 g of mixed aggregate
and ller were heated inside oven with temperature of 160 C for
3 h. Asphalt cement was also heated at 130 C to be suitable for
mixing with aggregate particles. All the materials were mixed at
the temperature of 160 C. PET particles with different percentages
(0%, 0.5% and 1% by weight of aggregate particles) were added
directly to the mixture as the method of dry process. The loose
mixture was compacted using Marshall compactor and 50 blows
of compaction efforts were applied on each side of the mixture.
It is worth mentioning that all the mixtures were fabricated at
their optimum asphalt contents (OAC). The optimum asphalt content for SMA mixtures is usually selected to produce 35% air voids
[4,5]. In this study, the OAC was selected to produce 4% air voids.
The summary of the mix design is reported in Table 2.
2.2. Indirect tensile stiffness modulus test
Indirect tensile stiffness modulus (ITSM) test gives the relationship between stress and strain of asphalt mixture and used to evaluate the stiffness of asphalt mixture at specic environmental
conditions. ITSM test was performed in accordance with AASHTO
TP31. ITSM test can be performed by using Universal Testing
Machine (UTM) which is one of the important testing equipment
in pavement laboratory. UTM is a computer controlled system
which operates automatically. During the test, compressive

120

100

haversine waveform loads were applied across the thickness of

specimen, and by utilizing Linear Variable Differential Transducers
(LVDTs) which were installed along diametrical section of specimen displacement of asphalt mixture was measured. Horizontal
tensile stress and stiffness modulus of asphalt mixtures was calculated using the following equations [10,16]:

rx max
Sm

2P

pdt

P  m 0:27
Ht

where rx(max) is the maximum horizontal tensile stress in middle

of specimen (kPa); Sm is the stiffness modulus (MPa); P, applied vertical peak load (N); H, amplitude of horizontal deformation (mm); t,
average thickness of specimen (mm); d, average diameter of specimen (mm) and m, Poissons ratio.
In order to characterize effects of applied stress and temperatures
on the mixtures stiffness, ITSM test was conducted at stress levels of
200, 300 and 400 kPa for each percentage of PET which are the stress
amounts mostly used at pavement laboratories. Additionally, testing temperatures of 10 C, 25 C and 40 C were designated which
can be referred to relatively low, medium and high environmental
temperatures respectively.
2.3. Method of analysis
One factor at a time (OFAT) methodology is a conventional
approach to optimize multifactor experiments. OFAT includes a
changeable single factor for a specic experiments design while
other factors are kept constant. OFAT is unable to provide appropriate output because the effect of interactions amongst all
involved factors in the designs is not examined truly, and it is
not capable of reaching the true optimum value [17,18]. Hence,
RSM methodology was introduced for parameter optimization in
a way that number of experiments and interaction among the
parameters are reduced to minimal value [1921]. Consequently,
the Design Expert 8.0.5 was designated for this study to generate
statistical analysis, experimental designs, and to calculate the sorbent adaption conditions.
For this study, a developed quadratic model and a = 0.5 were
utilized using RSM method for design and data analyzing. In this
investigation, the effects of three independent numerical variables

Lower limit
Upper limit
Design limit

Passing (%)

80

60

40

20

0
0.075

0.3

0.6

2.36

4.75

Sieve size (mm)

Fig. 1. Aggregate particle size distribution for stone mastic asphalt.

9.5

12.5

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T. Baghaee Moghaddam et al. / Materials and Design 68 (2015) 8896

Table 1
Properties of materials.
Property

Unit

Used specication

Value

Requirements

Asphalt
Penetration at 25 C
Softening point
Flash point
Fire point
Specic gravity

0.1 mm
C
C
C
(g/cm3)

ASTM:
ASTM:
ASTM:
ASTM:
ASTM:

D5
D36
D92
D92
D70

87.5
46.6
300
320
1.03

Coarse aggregate
L.A. Abrasion
Flakiness index
Elongation index
Aggregate crushing value
Bulk specic gravity
Absorption

%
%
%
%
(g/cm3)
%

ASTM: C131
BS 812 Part 105.1
BS 812 Part 105.2
BS 812 Part 3
ASTM: C127
ASTM: C127

19.45
2.72
11.26
19.10
2.60
0.72

<30
<20
<20
<30

<2

Fine aggregate
Bulk specic gravity
Absorption
Soundness loss

(g/cm3)
%
%

ASTM: C128
ASTM: C128
ASTM: C88

2.63
0.4
4.1

<2
<15

Table 2
Summary of mix design.

a
b
c
d

PET (%)

BSGa

VMAb (%)

VFAc (%)

OACd (%)

0
0.5
1

2.294
2.296
2.283

18.12
17.34
17.55

77.92
76.90
77.20

6.77
6.36
6.51

xi describes the coded value of the ith independent factor which is

dimensionless. Actual value is dened as Xi, X0 is the center point
actual value and DX refers to the step change of the ith variable.
Totally 34 experiments in randomized order were performed,
together with ve replications at center points to provide accurate
assessment of errors (Table 3). The stiffness was dened as the
response to develop design of experiment modeling. Eq. (4) was
introduced to calculate the dependent variables [22,23]:

Y b0

n
n
n X
n
X
X
X
bi xi
bii x2i
bij xi xj e
i1

i1

SSresidual =DF residual

SSmodel SSresidual =DF model DF residual

In this equation, SS is the sum of squares and DF is degrees of

freedom.
Eqs. (7) and (8) and an F-test in the program were used to check
the models adequate precision ratio (AP) to determine the statistical importance of the model [2426]:

including PET modier (A) from zero to 1%, stress levels (B) from
200 kPa to 400 kPa and temperatures (C) between 10 and 40 C,
all at three levels, were studied through the Central Composite
Design (CCD). Related literature and preliminary studies were used
to choose these variables and the irrespective regions of interest
[58,1012].
Table 3 shows the levels and range of the actual values of independent numerical variables. By using Eq. (3) all dened numerical
variables transformed to the coded form.

X i  X 0
DX

SSresidual
SSmodel SSresidual

R2adj 1 

Bulk specic gravity of compacted mixture.

Void in mineral aggregate.
Void lled with asphalt.
Optimum asphalt content.

xi

R2 1 

i1 j1

In the Eq. (4), Y is the calculated response, b0 is the constant. Independent variables in coded forms are described as xi, and xj. The
coefcients of bi and bii are the linear and quadratic terms. bij is
the interaction term coefcient, e is the random error, and the studied number of factors is described as n.
Besides, in order to assess appropriateness of the proposed
model, analysis of variance (ANOVA) was performed. The coefcients of determination (R2 and R2adj) express the wellness of the
t to suggested model. These values can be determined using the
following equations [24,25]:

Adequate Precision

VY

maxY  minY
p
V Y

n
1X
pr2
VY
n i1
n

where Y is the predicted response, p represents the number of

model parameters, residual mean square is described as r2, and n
is the number of experiments.
After the F-test had been performed, the insignicant terms
were found and eliminated from the model. Thereafter, the nalized model was introduced based on the signicant variables.
Eventually, the optimum condition was determined to give the
highest stiffness response, along with better mixture performance.
3. Results and discussion
Indirect tensile stiffness modulus test was conducted on the PET
modied SMA mixtures at elevated temperatures and stress levels.
Table 3 represents the layout for experimental design and the
amounts of stiffness responses. Having these values, RSM was utilized to nd interactions between the outputs and variables which
are independent. Eventually, a tted quadratic polynomial equation was produced after a regression analysis had been applied to
all responses described in the design matrix. The highest order
polynomials with signicant model performance are suggested
by the software. This model was utilized to nd the optimum
condition. The numerical parameters (A, B and C) were used to
generate the predictive model according to Eq. (9):

Final Equation for Stiffness 4051:55  325:25A  171:5B

 4776:15C 256:75AC  157:96A2 1602:54C 2

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T. Baghaee Moghaddam et al. / Materials and Design 68 (2015) 8896

Table 3
Layout of experimental results and DOE design.
Run

Factor 1: PET (%)

Factor 2: stress level (kPa)

Factor 3: temperature (C)

Stiffness (MPa)

1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34

0
1
0.5
0
1
0.5
0.5
0.5
0
0.5
1
0
1
0
0
0.5
0.5
1
0.5
0
1
1
0.5
0.5
0
0.5
1
0.5
1
0
0.5
1
0.5
0

200
400
300
200
300
300
200
400
300
300
400
300
200
400
200
300
300
400
300
400
200
300
300
300
400
300
400
400
200
400
200
200
300
200

10
40
10
40
25
25
25
25
25
25
10
25
10
10
40
25
25
40
25
40
10
25
40
40
40
10
10
25
40
10
25
40
25
10

10,801
452
10,608
1011
3689
4088
4310
3758
4041
4083
9391
4083
9710
10,762
1071
4025
4081
431
4022
632
9712
3722
645
623
664
10,701
9410
3671
832
10,769
4261
821
4089
10,841

Table 4
Anova analysis for stiffness.
Source

Sum of squares

Degree of freedom

Mean square

F value

Prob > F

Model performance

Model
A
B
C
A2
B2
C2
AB
AC
BC
Residual
Lack of t (LOF)
Pure error
Cor total

478763078.9
2115751.25
588,245
456232176.5
133703.7816
9322.861812
13761302.46
15252.25
1,054,729
42,436
486333.2542
466621.9209
19711.33333
479249412.1

9
1
1
1
1
1
1
1
1
1
24
5
19
33

53195897.65
2115751.25
588,245
456232176.5
133703.7816
9322.861812
13761302.46
15252.25
1,054,729
42,436
20263.88559
93324.38418
1037.438596

2625.158
104.4099
29.02923
22514.55
6.598131
0.460073
679.1048
0.752681
52.04969
2.094169

<0.0001
<0.0001
<0.0001
<0.0001
0.0169
0.5041
<0.0001
0.3942
<0.0001
0.1608

Signicant
Signicant
Signicant
Signicant
Signicant
Insignicant
Signicant
Insignicant
Signicant
Insignicant

89.95654

<0.0001

Signicant

Adequate precision (AP)

Checking the adequacy of the model is an important part of the

data analysis, as the model functions would give improper
responses in case the t is not adequate [20,27]. Hence, in this
study in order to assess the signicance and adequacy of the model
ANOVA analysis was performed and the results are reported in
Table 4. In addition, this table shows the quadratic models for
coded factors, and represents the other statistical parameters for
stiffness response. In this table, p-values which are less than
0.0001 imply that the model and parameter are signicant (model
and term p-value < 0.05 indicate the model and the term are significant for 95% condence intervals) for assessing the value of
responses [28].

136.602

In this study, the effect of PET (A), on stiffness property of SMA

mixtures at different stress levels (B) and temperatures (C) is modeled. Besides, in order to improve the model performance, insignificant terms (with p-value > 0.100) are eliminated from the model
[29].
In order to check the tness of the model, regression coefcients, R2 and R2adj were calculated. Values of 0.9990 and 0.9986 were
obtained for the R2 and R2adj, respectively. This shows that 99.8% of
the total variation in the stiffness response could be explained by
the quadratic model. The high R2 and adjusted R2 values indicate that
there is a good agreement between predicted and actual values
[21,22,30]. Ratio of signal-to-noise is measured by adequate

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T. Baghaee Moghaddam et al. / Materials and Design 68 (2015) 8896

Fig. 2. Design-expert plot; predicted versus actual values plot for stiffness.

precision to compare the variety of the estimated amounts at the

design points to the average prediction error. Adequate model discrimination was found in this study when the adequate precision
ratio of 136.602 was calculated for the stiffness which is much
higher than the value of 4 [31]. The lack of t (LOF) F-test was also
used to evaluate the adequacy of the model. LOF depicts the variation of the data around the tted model, and the amount of LOF
would be signicant if the model does not t the data well. It is
worth noting that despite the lack-of-t was signicant, the reasonable agreement between the predicted and adjusted R2 were found
for all responses which can be concluded the suggested model for
all responses can be used to navigate into design space to nd an
optimum condition [32,33].
3.1. Statistical analysis
In order to have better understating about model satisfactoriness, diagnostic plots such as the predicted versus actual values

are worthwhile. Fig. 2 shows the actual versus predicted values

plots of parameters removal for stiffness modeling. As it is depicted
in this gure there is an adequate agreement between the actual
data amounts and the predicted ones. The same thing can be
achieved from AP value (AP > 4) for the stiffness responses (see
Table 4). This veries that predicted model can be used to navigate
the design space dened by the CCD.

3.2. One factor analysis

One factor analysis is changing one factor at a time method.
That is to say, in this method a single factor is varied while all other
factors are kept constant for a particular set of experiments. And
this process exists for optimizing other variables which would be
time consuming. In this method, trial and error are commonly
existed for the optimization of variables, and, moreover, there is
always a lack to reach a true optimum amount which should be

Fig. 3. Effect of PET percentage on the stiffness.

T. Baghaee Moghaddam et al. / Materials and Design 68 (2015) 8896

93

Fig. 4. Effect of different stress levels on the stiffness.

obtained by considering the interaction among all the variables

[32,34].
Each factor in this analysis is evaluated separately. Fig. 3
reveals the effect of PET on the stiffness properties of SMA mixtures. As it can be seen in this gure the amount of stiffness is
decreased at higher PET contents. The possible reason for this
result might be due to the mechanical properties of PET particles
in the mix. In fact, because the melting point of PET is a high (over
250 C) and is higher than the mixtures fabrication temperature,
the PET particles do not melt during mixing. The solid PET
particles can make mixture more exible and cause higher deformation under loading application. The same pattern is found
between stress level and stiffness value as it is depicted in
Fig. 4. That is to say, by increasing the stress level, the amount
of deformation in the mixture is increased and according to Eq.
(2) the stiffness is reduced mutually. Moreover, in Fig. 5, the
higher decreasing slope line may imply that the temperature variation has dominating inuence on the stiffness property of SMA

mixtures, and this represents the importance of ambient temperature on the stiffness property of asphalt mixture.
3.3. Effects of temperature and stress levels on the stiffness
The quadratic model for the effect of stress level and temperature on stiffness is presented in Fig. 6. The response was generated
using the Eq. (9). Fig. 6 shows that by variation of temperature
from 10 C to 40 C the amount of stiffness is decreased, however,
the effect of stress seems to be negligible compared to the temperature variation.
3.4. Effects of temperature and PET content on the stiffness
Effects of two parameters including PET and temperature are
evaluated on stiffness as shown in Fig. 7. Fig. 7 depicts the mixture
stiffness is more susceptible against variation of temperature. The
stiffness amounts decrease from over 10,000 MPa to under

Fig. 5. Effect of different temperatures on the stiffness.

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T. Baghaee Moghaddam et al. / Materials and Design 68 (2015) 8896

Fig. 6. Effects of stress level and temperature on the stiffness, 0.5% PET.

Fig. 7. Effects of PET percentage and temperature on the stiffness, stress level 300 kPa.

1000 MPa when the temperature increases from 10 C to 40 C.

Additionally, it is shown at lower temperatures the PET amounts
have more inuence on the mixture stiffness. This can be referred
to susceptibility of asphalt binder against temperature variation
which plays an important role on the mixture properties. In other
words, when the ambient temperature increases, the asphalt binder becomes soft which can eventually results in lower mixture
stiffness. Besides, the inuence of PET on mixtures stiffness is
overshadowed by the temperature.
3.5. Effects of PET and stress level on the stiffness
Fig. 8 shows the effects of stress level and PET on the stiffness of
asphalt mixture. It might be realized that both level of stress and
PET content have nearly the same effect on stiffness property of
asphalt mixture though the variation of PET might be more inuential, for instance at 400 kPa by increasing the PET amount from
0% to 1% the stiffness value decreases by 378 MPa.

3.6. Finding the optimum condition

In the construction of asphalt mixture, relatively high stiffness is
demanded to resists against trafc loading and consequently permanent deformation. Optimum PET content for maximizing the stiffness within the considered experimental range was accomplished
using the Design-Expert software. An overlay plot is used to view
constraints on process or formulation. The optimum conditions
could be graphically visualized by super imposing the contours of
the response surfaces in an overlay plot. As depicted by Fig. 9,
0.41% of PET is suggested by the software to provide the highest stiffness value.
4. Conclusions
This paper aimed to evaluate the effects of applied load and temperature on the stiffness property of unmodied and PET modied
asphalt mixtures. Statistical analysis was used in this investigation

T. Baghaee Moghaddam et al. / Materials and Design 68 (2015) 8896

95

Fig. 8. Effects of PET percentage and stress level on the stiffness, 25 C.

Fig. 9. Design-expert plot; overlay plot for optimal amount of PET.

to nd interactions between selected variables. A good agreement

was found between predicted and actual values. A quadratic model
was successfully tted to the experimental data. Based on the results
achieved in this study the following conclusions can be derived:
(1) Stiffness of asphalt mixture was affected by amounts of
applied stress and PET content. However, mixture stiffness
was more susceptible against temperature variations.
(2) The results showed that the PET modication had more inuence on the asphalt mixtures stiffness at lower temperatures.
(3) The ndings of this study revealed that the variation of PET
was more inuential on the stiffness of mixtures compared
to the stress levels.
(4) 0.41% of PET content was selected as the optimal PET value
to reach the highest stiffness for the SMA mixtures which
have been designated for this study.

Acknowledgements
The authors express their sincere thanks for the funding support they received from the Ministry of Higher Education, Malaysia, Grant No: FP021-2011A and University of Malaya Grant No:
RP010A-13SUS.
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