INTERNATIONAL JOURNAL OF CIVIL AND STRUCTURAL ENGINEERING

Volume 5, No 2, 2014
© Copyright by the authors - Licensee IPA- Under Creative Commons license 3.0
Research article ISSN 0976 – 4399

Effects of exposure time and temperature in aging test on asphalt binder

properties
Engin Yener1, Sinan Hınıslıo lu2
1- Department of Civil Engineering, Bayburt University, Bayburt, Turkey
2- Department of Civil Engineering, Zirve University, Gaziantep, Turkey
eynr@yahoo.com
doi: 10.6088/ijcser.2014050011

ABSTRACT

The effect of temperature level and its exposure time in hot mix asphalt production stages on
the conventional and rheological properties of asphalt cements have been investigated
through experimental study. A series of Rolling Thin Film Oven (RTFO) Test was conducted
at the temperature/time combinations for 135, 150, 163 ºC and 40, 80, 120 minutes. Dynamic
mechanical characteristics of the binders were detected by dynamic shear rheometer tests.
The results show that the variations in exposure time and temperature distinctly changed the
properties of binders in a wide range. It is recommended that for a better simulation of short
term aging in production and construction stages, RTFO test temperature and curing time
should be adjusted according to the real individual field conditions. Also, in order to give
information about the aging behavior of a specific binder for possible field conditions, the
test results should be presented for a number of temperature-time combinations.

Keyword: Asphalt, pavement, short term aging, durability, rheology, aging test.

1. Introduction

Hot mix asphalts (HMA) should satisfy enough stability, durability, impermeability,
flexibility, coefficient of friction and workability for a good pavement performance. To
produce a mixture having these properties, a suitable coating of the aggregate grains by
asphalt binder and a suitable compaction up to designated air void ratio should be guaranteed.
The deficiencies in mixing process result in problems in the following processes of HMA
production (placement and compaction) and also in the performance of HMA through its
service life. Asphalt plant mixing temperatures for different binder grades have a wide range
as from 116°C to 171°C (APEC, 2000), Additionally, the mixing temperatures of modified
binders may be beyond 177°C according to the viscosity based mixing temperature
determination methods (West et al., 2010), Also the gradation and the surface texture of
aggregates changes the needed mixing temperature to coat the aggregate grains properly
(Yener and Hinislioglu, 2011), In addition, a proper mixing can be performed at these
temperatures with a rational mixing effort. The mixing duration and the mixing temperature
should not be higher than the needed for proper coating and workability, because, asphalt
binders are critically hardened in the production stages of HMA (Lee et al., 2009: Navarro et
al., 2009),

Two types of age hardening namely short-term and long-term aging occur through production
stages and service life of asphalt pavements. Short-term aging originates from hot mix asphalt
production, hauling and placement stages. Long-term aging originates from environmental
factors and traffic loads through the service life. Many kind of asphalt pavement deficiencies
like low temperature cracking, fatigue cracking, raveling, potholes originates from the lack of

Received on June, 2014Published on November 2014 112

 Effects of exposure time and temperature in aging test on asphalt binder properties
Engin Yener, Sinan Hınıslıo lu

enough flexibility, cohesion or adhesion which are directly or indirectly related to the binder
aging.

Heat, air, moisture and sun light are the main factors which changes negatively engineering
properties of the asphalt binders (Wu et al., 2008), These changes arise from different kinds
of binder aging as volatilization, oxidation, thixotrophy, syneresis and polymerization.
Moving away the lighter ingredients in asphalt cement refer to volatilization which is mainly
a function of temperature and take place mostly throughout production stages. Oxidation
hardening that changes lighter oil molecules to maltene and maltene to asphaltene is caused
from chemical reaction between the hydrocarbon compounds of bitumen and oxygen
(Whiteoak, 1990: Hunter, 1994: Ali et al., 2008), Volatilization and oxidation causes
irreversible hardening. A lattice structure formation of hydrophilic suspended particles causes
a reduction of rheological properties of the binder’ colloidal system refers to thixotrophy.
Thixotropic hardening can be reversed by heat and agitation (Soltani and Anderson, 2005),
Syneresis (oil exudation) is the separation of less viscous compounds from the more viscous
molecular network of asphalt cement. Colloidally unstable bitumens can potentially exhibit
syneresis problems (Oliver, 2009), This event causes physical or chemical alterations in
molecular structure of binder. Polymerization is the coming together of similar molecules to
form larger molecules which cause a progressive hardening. High ratio volatilization and
oxidative hardening occurs during the mixing process in the asphalt plants because thin
asphalt binder films are exposed to air at high temperatures. If the mixing continues too long
and/or the temperature is very high the aging occurs severely. Also total passing time until
compaction is important due to the high hardening potential of binder in loose asphalt
mixture with high void ratio at high temperatures.

Traxler (1963) listed a number of effects which may reduce the binding properties of asphalt.
This study showed that time and heat parameters are the reason of many aging factors. The
effects of different levels of mixing time and mixing temperature on asphalt aging have been
studied using varying methods in literature (Lee, 1973: Kim et al., 1986: Mallick and Brown,
2004: Lee et al., 2009: Wu et al., 2009: Yu et al., 2009),

Mallick and Brown (2004) recovered asphalt binders from both loose mixtures in production
stages and one-year, two-year and three-year core samples after production. Furthermore,
they produced laboratory samples aged in RTFO and pressure aging vessel (PAV), Finally,
bending beam rheometer (BBR) and dynamic shear rheometer (DSR) tests were conducted
for comparison purposes. Complex shear modules (G*), phase angle ( ), fatigue factor
(G*sin ) and low temperature stiffness (S) values is evaluated in the study. The results
showed that PAV test is capable of simulating long term aging. Taken RTFOT, statistical
analysis results show that there is no significant difference between the results of recovered
asphalt cements and RTFOT binders (p=0.9735),

Wu et al. (2009) investigated the changes in structural, morphological and rheological

properties of raw and SBS modified binders due to aging. In their study, RTFO (75 min,
163 °C, air flow at 4 L/min) and PAV (at 60 °C, test duration from 600, 1200 to 2000 h) tests
were conducted as laboratory simulation aging methods. Asphalt binder properties were
investigated by Fourier transform infrared spectroscopy, softening point, DSR and atomic
force microscopy. It was reported that the raw bitumen and modified asphalts showed similar
rheology and mechanical characteristics after age hardening.

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Yu et al. (2009) investigated the effects of organo-montmorillonite on thermo-oxidative and

ultraviolet aging properties of asphalt. Thin-film oven (TFO) and PAV test were conducted as
aging tests. Viscosity aging index (VAI) and softening point increment, ductility retention
rate and DSR test results (rut factor (G*/sin ) after TFOT, fatigue factor (G*sin ) after PAV)
were evaluated in the study. Results show that organo-montmorillonite increased short term
aging resistance.

Lee et al. (2009) investigated the effects of the short-term oven aging (STOA) on asphalt
mixtures, by the combinations of two temperatures (135 and154 °C) and three duration times
(0, 2 and 4 h), Aging is evaluated using the gel-permeation chromatography test procedure.
Results show that increasing aging temperature and curing time increased the large molecular
size (LMS) ratio. However, effect of binder type (un-modified, SBS-modified, rubber-
modified) on aging of asphalt mixtures was not statistically significant. Also, it was reported
that RTFO has less aging effect than any STOA used for the asphalt mixtures according to
the LMS ratios. Nevertheless, the effects of aging temperature and curing time conditions on
binder rheology weren’t investigated.

In this study, in order to show more clearly the effect of mixing time and mixing temperature
variations on the effect of asphalt rheology, conventional asphalt tests and dynamic
mechanical tests were performed on the aged and un-aged asphalt binders. To simulate the
aging in field mixing process the RTFOT was conducted at the combinations of three aging
temperatures (135, 150, 163 ºC) and three curing times (40, 80, 120 min), The results showed
that the aging time and aging temperatures distinctly changed asphalt binder properties.
Eventually, it is concluded that a fixed aging temperature at 163 °C and curing time as 85 min
in the RTFOT is not the best approach to simulate short term aging. As a better way, it is
proposed to adjust the RTFO test temperature according to the real mixing temperatures and
to adjust the curing time according to the asphalt plant, hauling distance and the other
conditions for a specific construction.

2. Materials and methods

An un-modified asphalt binder with a penetration grade of B50/70 obtained from Batman
refinery in Turkey was used in this study. The characteristics of original binder were shown in
Table 1. Also, original binder samples were aged at the combinations of three temperatures
(135, 150 and 163°C) and three aging times (40, 80 and 120min.s) in RTFOT. After RTFOT,
loss of weight, penetration, softening point and dynamic rheological parameters were
determined for every conditioned binder. The aging procedure and the other test methods
which were carried out to determine the binder properties are explained below. Figure1 shows
a flow chart of the experimental design procedure.

Table 1: The physical properties of the original asphalt binder used in this study
Test Test Result Standard
Penetration @ 25 °C
68 ASTM D 5-73
(0.1mm)
Ductility @25 °C (cm) >100 ASTM D 113-79
Weight Loss (%) 0.05 ASTM D 6-80
Specific gravity @ 25°C
1.029 ASTM D 70-76
(g/cm3)
Softening Point (°C) 49 ASTM D 36-76
Flash Point (°C) 298 ASTM D 92-78

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2.1 Rolling thin film oven test

RTFOT is a modified form of Thin Film Oven Test (TFOT) to eliminate the surface limited
aging. In RTFOT, asphalt binder is filled in cylindrical glass bottles and the bottles are rotated
at horizontal axis. Thus, a homogeny aging can be ensured. In this test, asphalt film thickness
is lowered to 1.25 mm, so the mixing process in asphalt plant is simulated better than in the
TFOT. RTFOT apparatus have a rotary carriage on a horizontal axis with a capacity of 8 test
bottles. Rotational speed of the carriage is 15 rpm. Also, approximately 35g asphalt sample is
filled in a test bottle. During the standard test process, the oven temperature is 163ºC, the test
time is 85 min. and the airflow into the bottles is 4000 ml/min. In this study, test temperature
and test time were changed to the combinations of 135ºC, 150ºC, 163ºC and 40 min, 80 min,
120 min. In 1970, RTFOT were accepted as a standard test method by ASTM to evaluate the
effect of heat and air on a moving film of asphalt (ASTM D2872),

Figure 1: Flow chart of experimental procedure

2.2 Penetration test

The penetration is an empirical test which is widely used to determine the consistency and
grade of asphalt binders. The standard test procedure is described in ASTM D5. In the test, a
needle with 100 g total weight is installed on to the asphalt sample at 25 °C for 5 seconds. The
penetration level of the needle is measured and reported in units of 0.1 mm (Tia, 2002), Softer
asphalt cements have higher penetration values than harder ones. Some transportation agencies
use the penetration test results to classify the asphalt cement grades (TS 1081 EN 12591),
Asphalt cement with B50/70 penetration grade was used in this study.

2.3 Ring & ball softening point test

The softening point is defined as the temperature at which an asphalt sample can no longer
bear the weight of a standard steel ball. In this test, an asphalt sample is filled in a metal ring.
The dimensions of the ring are 15.875 mm inside diameter by 2.38 mm thick by 6.35 mm deep.
This ring is placed on a test stand in a heating bath, and the steel ball having weight of 3.5gr is
placed on the asphalt specimen. The softening point temperature of asphalt cement is written

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down when the ball penetrates the specimen and reaches the standard distance. This test was
executed according to ASTM D 36.

2.4 Temperature susceptibility

The hardening caused by aging increases stability of asphalt binder and asphalt mixture, but
decreases adhesion and a fragile structure come into existence especially at lower temperatures
and under dynamic load conditions. Asphalt binders having high temperature susceptibility are
unwanted as pavement construction material. Penetration Index (PI) is frequently used to
comment the susceptibility of bitumen to temperature changes. An asphalt cement with a very
high temperature susceptibility can be have a low PI value as -3, while an asphalt with a very
low temperature susceptibility can be have a high PI value as +7. It is highly possible that high
temperature susceptible asphalt will cause low stability at high temperatures, and it will cause
a fragile structure at low temperatures. It means that an asphalt binder with low PI does not be
able to resist to rutting in hot climate regions. In addition to this, it shows a brittle behavior
resulting in alligator cracking or fatigue cracking in cold days. The pavements produced with
such asphalt binders deteriorate in early stages of their service life. Thus, asphalt binders with
low PI values which mean high temperature susceptibility are undesirable. PI can be
calculated using equation (1) and (2), if we know softening point (TRB) and standard
penetration at 25°C (Pfeiffer and Van Doormal, 1936), It is assumed that the penetration value
at the temperature of softening point is 800 (Ulliditz, 1987),
A = [log800 – log (P25)] / (TRB – 25) (1)
PI = (20 – 500A) / (1 + 50A) (2)

PI values were calculated for original asphalt and the aged asphalts which are hardened in
RTFOT at varying time-temperature combinations. PI values were shown in Table 2.

2.5 Rheological analyses

Bohlin Dynamic Shear Rheometer (DSR) is used in this study to determine rheological
properties of aged and un-aged asphalts. For this aim, viscosimeter tests and oscillatory tests
were conducted with DSR. In these tests, thin asphalt samples in the dimensions of 1 mm
thickness and 25 mm diameter were used as shown in Figure2. Parallel plate viscosimeter tests
were conducted varying shear rates from 0.1 sec-1 up to10 sec-1 at 60 °C to find the relation
between shear rate and dynamic viscosity, and also to see the effect of aging time and
temperatures on viscosity. Viscosity ( ) values (at 60°C and 0.4 sec-1 shear rate) and Aging
Index (AI) values [( aged- unaged)/ unaged] were given in Table 2.

DSR oscillation tests were performed to detect complex shear modulus (G*) and phase angle
( ), In this test base plate is stationary and the spindle moves backwards and forwards
generating shearing action (Figure2b), Time lag between the maximum applied stress ( max)
and the maximum shear strain ( max) is the phase angle ( ) (see Fig.2), Complex shear
modulus is the ratio of max to max. G* has elastic and viscous components due to viscoelastic
behavior of asphalt binders. Elastic part (G’) is G*cos , and viscous part (G”) is G*sin . For
rutting resistance, high G* and small values is wanted at elevated temperatures. For fatigue
resistance, small G” values is wanted at service temperatures. In this study, in order to observe
the possible behavior of aged and un-aged binders at cold, medium and hot weathers,
oscillation tests were conducted varying temperatures from 10 °C up to 60 °C. Thus, dynamic
rheological parameters (G*, , G’, G”) were determined.

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Figure 2: Dynamic Shear Rheometer modules: (a) viscosimeter mode (b) oscillation mode

Figure 3: The effect of aging time and temperature on the volatilization

3. Results and discussion

3.1 Conventional test results

According to the weight loss, penetration and softening point test results, effect of aging
conditions on asphalt binder properties were presented graphical form in Figure3-5. Loss of
weight after aging test is a proper indicator of hardening caused by volatilization. As shown in
Figure3, increasing the duration and the temperature in RTFOT linearly increased the weight
loss. Thus, it can be said that the volatilization based hardening significantly increased after
short term aging. RTFOT curing time increases the volatilization at high temperatures more
than the low temperatures.

Penetration value gives information about the performance of binder in general service
conditions and at average ambient temperatures. Increasing the test duration and the test
temperature in RTFO caused a decrease at penetration values, as shown in Figure 4. Softening
point of asphalt binder gives information about the stability of pavement in hot days. The most
important problem which is commonly encountered is the rutting distress. The effect of aging

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time and aging temperatures on the softening point of the binder was shown in Figure 5. It can
be seen that increasing aging time and temperature increased the softening point. In this
situation, the pavement with asphalt which is highly hardened during the production process
will be more resistant to the rutting distress. This is a favorable advantage of the short term
aging mentioned in literature (Vallerga, 1981), However, it should be considered that aged
asphalts are more brittle and susceptible to the fatigue cracking in cold weathers.

Figure 4: The effect of aging time and temperature on the penetration

Figure 5: The effect of aging time and temperature on the softening point

Table 2: Penetration index and aging index values of virgin binder and aged binders
150° 163° 163°
150°C
Aging 135°C 135°C 135°C 150°C C C C 163°C
Unaged 120mi
conditions 40min 80min 120min 40min 80mi 40mi 80mi 120min
n
n n n
Penetration
-0,61 -1,05 -0,98 -0,83 -1,04 -1,08 -0,99 -1,27 -0,98 -0,37
index
PI 0,00 -0,45 -0,37 -0,22 -0,43 -0,47 -0,38 -0,66 -0,38 +0,24
Aging
0 25 26 68 127 122 369 125 306 758
index (%)
sec-1
* Based on the viscosity values at 60°C and 0.4 shear rate, aging Index was calculated as AI=
( aged- unaged)/ unaged.

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The effect of temperature-time combinations in the aging test on the temperature susceptibility
(penetration index) of the asphalt was shown in Table 2. It can be seen that aging caused a
decrease in PI for the selected temperature-time combinations except for 163ºC-120min. The
increase of PI in the condition of 163ºC-120min should not been considered as an
improvement, since the hardening at 163ºC-120min is very high (see Figure3-4), The worst
temperature susceptible binder among them was the binder aged temperature-time
combination of 163ºC-40min with the least PI value (-1,27),

Figure 6: Shear rate-viscosity curves of the aged and un-aged binders

3.2 DSR tests

3.2.1 Viscosity test results

Figure6 shows the relationship between the dynamic viscosity and the shear rate for the un-
aged binder and the aged binders. Dynamic viscosities increased as the aging time and aging
temperatures increased. This suggests that the exposure time and temperature conditions affect
the flow behavior of the binders, which may be due to the changes in the molecular structure
of bitumen by aging. Also, viscosity values of the binders decreased as shear rate is increased.
This shear thinning behavior is clearer for the binders which were aged longer time at higher
temperatures. The shear thinning implies that the age hardening shifts the linear viscoelastic
range of the asphalt cements towards higher temperatures.

Figure 7: Effect of aging conditions on aging index

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In order to show more clearly the effect of time and temperature variations on the changes in
viscosity, aging index vs. time relationships for every temperature were drawn in Figure7.
Results show that longer aging time at low temperatures is not so harmful (at 135 ºC), but it is
very detrimental at high temperatures, particularly at 163 ºC. Assuming the exposure time in
RTFOT is representative of mixing time in an asphalt plant, it can be seen from Table 2 and
Figure7, 1.5 fold increase in mixing time (from 80 min to 120 min. at 163 ºC) has caused 2.5
fold increase in aging index (from %306 to %758), Also the viscosity of binder aged at 150 ºC
through 120 min. is higher than the viscosity of binder aged at 163 ºC through 80 min.

4. Oscillatory test results

A temperature dependence test (from 10 ºC to 60 ºC) was conducted to see viscoelastic

behavior of aged and un-aged binders. The loading frequency was selected as 10 rad/s (1.59
Hz), Thus, the complex modulus (G*) and the phase angle ( ) vs. asphalt temperature
diagrams were drawn for aged and un-aged binders (Figure8), From the graphs in Figure8, it
can be seen that aged binders behave in a different way, since an increase in G* values are
noticed at all test temperatures, yielding even higher values than those corresponding to un-
aged bitumen. This type of increase has negative effects on asphalt pavement performance at
low temperatures, because the stiffness of the binder is increased. Especially at low
temperatures, thermal cracking potential of pavement increases due to the lack of flexibility
(Lu et al., 2003), However, the increase in G* values has positive effects on binder
performance at high service temperatures, because increasing binder stiffness reduces
permanent deformation potential at hot weathers (Navarro et al., 2009),

4.1 Binder Rutting Parameter (G*/sin )

Traffic load repetitions cause cumulative permanent deformations in the pavement mixtures,
especially in hot weathers. This kind of pavement deterioration is named as rutting. Rutting
behavior of a pavement is related both asphalt binder properties and aggregate properties
(Arasan et al., 2011), Rutting resistance is more important at hot asphalt temperatures than low
temperatures. G*/sin values is considered as a numerical indicator of rutting resistance
(Anderson and Kennedy, 1993: Airey, 2004), Higher G*/sin values are favorable for
permanent deformation resistance. Rutting parameters at 60 °C and 40 °C for all binders were
calculated and presented in Figure9. Results show that increasing RTFOT curing time and
temperature increases rutting resistance.

4.2 Binder Fatigue Parameter (G*.sin )

In the situation of lack of flexibility, repeated traffic loads cause fatigue (alligator) cracking
which is counted as an important deterioration mode for HMA pavements (Abo-Qudais and
Shatnawi, 2007), G*.sin values at 10 rads/s and at medium temperatures is considered as a
numerical indicator of fatigue resistance (Anderson and Kennedy, 1993: Airey, 2004, Al-
Khateeb et al., 2009), Lower G*.sin values are favorable for better fatigue performance.
Fatigue parameters at 25 °C for all binders were calculated and presented in Figure10. Results
show that decreasing RTFOT curing time and temperature improved the fatigue performance.
This is expected and in harmony with literature like that Gandhi (2008) reported that some
binders which were produced at lower mixing and compaction temperatures than usual
showed better fatigue cracking performance.

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Figure 8: Effect of aging conditions on complex shear modulus, elastic modulus, viscous
modulus and phase angle at varying service temperatures

Figure 9: Effects of aging conditions on rutting resistance

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Figure 10: Effects of aging conditions on fatigue resistance

5. Conclusions

In the usual production of Hot Mix Asphalt (HMA), firstly asphalt binder and aggregate was
heated at elevated temperatures about 155ºC. Then aggregate and asphalt binder were mixed
until obtaining fully covered aggregates by binder. The results of this study showed that
aging time and heating temperature have significant effects on short term age hardening. To
protect the binder from harsh aging effects, mixing temperature and mixing time in asphalt
plant should not be higher than the needed for proper coating and workability. In addition,
current short term aging test temperature and curing time are fixed in the specifications as
163 ºC and 85 minutes, respectively (ASTM D 2872), However in the field, hot mix asphalt
productions are sometimes to be made at higher temperatures and longer mixing times to
properly coat aggregates with binder, especially in case of using modified binders. Also
needed mixing temperature and mixing time may be lower than usual in case of using warm
mix asphalt additives. Thus, for a better simulation of short term aging, RTFO test
temperature and curing time should be adjusted according to the real individual field
conditions. Also, asphalt binder manufacturers should provide information about the aging
behavior of a specific binder for possible field conditions. Therefore, aging test results should
be presented for a number of temperature-time combinations which have a range suitable to
the possible field conditions.

6. References

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Volume 5 Issue 2 2014