Construction and Building Materials 71 (2014) 451–455

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Construction and Building Materials

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The influence of water on the oxidation of asphalt cements

Jesús Alfredo Hernández Noguera a,⇑, Hugo Alexander Rondón Quintana b, Wilmar Darío Fernández Gómez b
a
Instituto de Ingeniería, Universidad Nacional Autónoma de México, Ciudad Universitaria, Coyoacán 04510, México, D.F., Mexico
b
Faculty of Environment and Natural Resources, Francisco José de Caldas District University, Avenida Circunvalar Venado de Oro, Bogotá D.C., Colombia

h i g h l i g h t s

 The interaction between water oxygen molecules and asphalt changes the asphalt properties.
 Increases in the asphalt stiffness and viscosity are observed after immersion in distilled water for one year.
 The consistency of the binder changes and its stiffness increases in the presence of water.
 Aging and oxidation are caused by the air–asphalt or air–water–asphalt interaction and by the oxygen from the water.

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

Article history: Two grades of paving asphalt, AC 80-100 and AC 60-70, were studied to determine changes in their phys-
Received 29 April 2014 ical and chemical properties caused by exposure to water. This experimental study’s primary hypothesis
Received in revised form 12 August 2014 is that the interaction between the water oxygen molecules and asphalt, known as oxidation, changes the
Accepted 23 August 2014
asphalt properties, resulting in increased damage from mechanisms such as humidity and aging for mix-
tures in service. The chemical responses of both asphalts were measured, and the flow activation energy
concept was used to understand the resulting changes in the physical and rheological properties after
Keywords:
immersion in distilled water for one year.
Asphalt cement
Oxidation
Ó 2014 Elsevier Ltd. All rights reserved.
Water influence
Flow activation energy

1. Introduction According to Brock [2], oxidation is the process of combining or

In a flexible pavement structure, the primary causes of damage
to asphalt mixtures in service include moisture, aging, oxidation,
fatigue and rutting [1]. In the literature, the damage to asphalts
caused by moisture and aging are correlated primarily with
changes in their physical properties when the binder is oxidized.
For example, when an asphalt ages or is oxidized, its viscosity
and stiffness increase. In addition, the damage to asphalts by mois-
ture and aging generates a decrease in the adherence between the
mineral aggregate and the binder, thus increasing the probability
of the occurrence of asphalt stripping. This type of damage also
causes a transformation from a ductile behavior to a fragile behav-
ior for the asphalt and the asphalt mixture, making them brittle
and susceptible to cracking.
⇑ Corresponding author. Address: Avenida Universidad 3000, Instituto de Ingen-
iería, Edificio 6, Ciudad Universitaria, Coyoacán 04510, México D.F., Mexico. Tel.:
+52 5556233600x8522.
E-mail addresses: JHernandezN@iingen.unam.mx (J.A. Hernández Noguera),
harondonq@udistrital.edu.co (H.A. Rondón Quintana), wfernandez@udistrital.edu.
co (W.D. Fernández Gómez).
causing the combination of a specific substance with oxygen. In
asphalt pavements, oxidation is generally associated with the reac-
tion between the asphalt and the oxygen in air and/or moisture. As
the temperature and the exposure time of the asphalt in air
increase, the oxidation rate and aging rate also increase. From
the perspective of pavement engineering, no studies have been
performed on the effect of the oxygen in water on the properties
and behaviors of asphalts because asphalt is considered to be a
material with extremely low permeability. However, oxygen is
an essential component of water. It can produce oxidation and
short- and long-term changes in the chemical and physical proper-
ties of asphalt, particularly when the asphalt layer that covers the
mineral aggregate is thin, such as in asphalt mixtures. Therefore,
the effects of water on the physical, chemical and rheological
properties of two types of asphalt cements (ACs), AC 80-100 and
AC 60-70 (AC 80-100 and AC 60-70 refer to ACs with American
Society for Testing and Materials (ASTM) D-5 penetration test val-
ues between 80 and 100 tenths of a millimeter and between 60 and
70 tenths of a millimeter, respectively), are evaluated in this study.
To evaluate these properties, the following tests were performed:
the penetration test (ASTM D-5), the softening point test (ASTM

http://dx.doi.org/10.1016/j.conbuildmat.2014.08.064
0950-0618/Ó 2014 Elsevier Ltd. All rights reserved.
452 J.A. Hernández Noguera et al. / Construction and Building Materials 71 (2014) 451–455
D-36), the ductility test (ASTM D-113), the absolute viscosity test
(ASTM D-2171), the viscosity test at 135 °C (American Association
of State Highway and Transportation Officials (AASHTO) T-316),
rheological characterizations at intermediate and high tempera-
tures using an AASHTO T 315-05 dynamic shear rheometer (DSR)
and column liquid chromatography to quantify the chemical com-
position of the asphalts through the determination of the saturate,
aromatic, resin and asphaltene (SARA) fractions in asphalt samples
immersed in distilled water for 12 months. The mathematical
parameter flow activation energy (Ef) is used in this study to esti-
mate changes in the physical properties of asphalt that are only
produced by chemical reactions. The flow activation energy is an
estimate of the energy required by the asphalt to produce a chem-
ical reaction. It is determined from the viscosity at the temperature
of the binder. Because the material is not performing mechanical
work in the proposed experiments, the estimated activation energy
corresponds to the chemical work that is generated by the oxygen
in the distilled water reacting with the asphalt molecules.
Khalid [3] concluded that oxidation, which has been considered
to be the dominant process in the deterioration of binders in
asphalt pavements, is an irreversible chemical reaction that
involves asphalt components and atmospheric oxygen. Bocci and
Cerni [4] suggested that the in situ oxidation mechanisms are
primarily dependent on an increase in temperature (which
increases the degree of oxygen diffusion and accelerates chemical
reactions), the exposure time, the thickness of the asphalt layer
exposed to the oxygen and the amount of the air flow. With respect
to the physical changes, laboratory results (e.g., [5,6]) have shown
that when asphalt oxidizes, the penetration and the ductility both
decrease and the softening and ignition point temperatures both
increase. From the mechanical and dynamic points of view, an
incremental change is observed in the modulus ratio after aging
or oxidation, which is primarily from asphalt hardening [7,8]. Sim-
ilarly, the chemical changes corresponding to the rearrangement of
the asphalt molecules from volatilization and oxidation effects
generate changes in the SARA groups [9]. SARA fractions are molec-
ular moieties that share an affinity with some solvents; oxidation
from reactions with air and moisture changes that affinity. The nat-
ure of the affinity is also affected by changes in temperature. An
increase in asphaltene moieties and the formation of carbonyl
and sulfoxide functional groups have been widely reported as indi-
cators of oxidation in asphalt cements [10,11]. Despite several
studies addressing the mechanisms associated with specific
asphalt oxidation and transformation during aging [12–15], the
phenomena are not fully understood. Asphalt oxidation is a com-
plex phenomenon not only because of the complex molecular com-
position of the asphalt cement but also because of the complex
reaction kinetics.
More information regarding advancements in the aging of
asphalts and asphalt mixtures is detailed in the studies of Rondón
[16] and Fernández et al. [10,17].
2. Materials and methods
2.1. Material characterization
The ACs were tested to obtain physical properties, parameters and rheological
characterization using a DSR (AASHTO T 315-05). The results of these tests are
shown in Tables 1–3. In Tables 2 and 3, the temperatures used in the evaluation
of the asphalts correspond to the performance grade (PG) method at high and inter-
mediate temperatures for selecting the appropriate binder for pavement perfor-
mance in terms of rutting and fatigue cracking, according to the AASHTO
Performance Graded Binder Specification (MP1).
2.2. Experimental phase
Sheets of AC 80-100 and AC 60-70, approximately 2 mm in thickness, were
immersed in distilled water for a period of time (t) of twelve months. This thickness
was the smallest thickness that could be produced in glass containers with a
rectangular area (30 cm  30 cm) and a height of approximately 1 cm. Ideally, the
production of sheets with smaller thicknesses may have been sufficient because
the effect of water occurs primarily on the asphalt surface. The water was distilled
to eliminate minerals and chemicals that may affect the results. In this way, the
chemical changes generated in the asphalt are primarily attributed to interactions
with the water, particularly with the oxygen molecules (oxidation). The water
was replaced on a weekly basis to prevent contamination or skewed results. Every
two months, the asphalt layers were removed from the distilled water to perform
the penetration test (ASTM D-5), the softening point test (ASTM D-36), the ductility
test (ASTM D-113), the absolute viscosity test (ASTM D-2171) and the viscosity test
at 135 °C (AASHTO T-316) to evaluate changes in consistency when immersed in
water. In summary, these tests were performed on samples at t = 0 (not immersed
or neat asphalt) and at t = 2, 4, 6, 8, 10 and 12 months (immersed). Three samples
were used for each test performed. A phase of rheological characterization was also
performed (AASHTO T 315-05) using a DSR on the immersed sheets of AC 80-100
and AC 60-70. The temperatures used in the rheological evaluation of asphalts cor-
respond to the PG method at high and intermediate temperatures for selecting the
appropriate binder for pavement performance in terms of rutting and fatigue crack-
ing, according to the AASHTO Performance Graded Binder Specification (MP1). In
the rheological tests, three samples for each temperature were used, and the shear
modulus and phase angle were measured ten times for each sample. These tests
were performed on samples at t = 0 (not immersed or neat asphalt) and
t = 12 months (immersed). Prior to the tests, the surfaces of the AC sheets were
carefully dried with tow. Subsequently, the AC was separated from its support with
a spatula. The absolute viscosity test (60 °C) and the Brookfield viscosity test at
135 °C were performed using a vacuum capillary viscometer and a rotational vis-
cometer, respectively. Each test used an independent sample, i.e., no AC samples
were reused. In the previously mentioned tests, the asphalts only experienced
changes in their physical properties from reactions or chemical work done by
water–asphalt interactions. Therefore, an Arrhenius mathematical expression [18]
was used to evaluate the chemical kinetics of the water–asphalt interactions in
the ACs. Using this equation and the laboratory results of the asphalt viscosity ver-
sus temperature tests, Ef, which represents the energy required to perform the
chemical work generated by the physical changes discussed in the following sec-
tion, was obtained.
To evaluate the chemical responses of the asphalts immersed in water for
12 months, which occur during the separation of the asphalt binder in asphaltenes
and maltenes by precipitation with n-heptane and subsequent fractionation of the
maltenes through an alumina column with solvents of increasing polarity, the SARA
fractionation test was performed according to ASTM D-4124 specifications. A
detailed description of this test, which was performed on both a non-immersed
(t = 0 or neat asphalt) sample and a sample immersed for t = 12 months, can be
found in the literature [19].
3. Results and discussion
Figs. 1–5 show the evolution of the penetration, softening point,
ductility and viscosity with immersion time of the ACs analyzed (AC
80-100 and AC 60-70). The asphalt penetration decreases with
immersion time in distilled water (refer to Fig. 1). At t = 12 months,
the penetration decreases by 26% and 34% for AC 80-100 and AC
60-70, respectively. This decrease in penetration corresponds with
the results obtained for the other measured parameters (increase in
the softening point and viscosity and decrease in the ductility).
At t = 12 months, increases in the softening points of 8% and 7%
are observed for AC 80-100 and AC 60-70, respectively. The
increases in viscosity for this immersion time are 20% and 31% at
60 °C and 40% and 38% at 135 °C for AC 80-100 and AC 60-70,
respectively; the decreases in ductility were 17% and 21%,
respectively.
Tables 4 and 5 show the results of the rheology tests per-
formed on the asphalts immersed in distilled water for 12 months.
Compared with the results shown in Tables 2 and 3 (non-
immersed asphalts), the shear modulus G* for AC 60-70 and AC
80-100 increased between approximately 5% and 15% when the
sheets were immersed in distilled water for 12 months. The
elastic component of the asphalts increased (shown by a decrease
in the phase angle d), which predicts that the asphalt elastic
response will increase more rapidly than the viscous response
from the presence of oxygen during the oxidation. The molecular
agglomerates lose mobility, the phase angle decreases, and the
viscosity increases, changes that are reflected in the rheological
properties [20–23].
 J.A. Hernández Noguera et al. / Construction and Building Materials 71 (2014) 451–455 453

Table 1
General characteristics of AC 80-100 and AC 60-70.

Test Method Units AC 80-100 AC 60-70

Tests on the original asphalt
Penetration (25 °C, 100 g, 5 s) ASTM D-5 0.1 mm 84 65
Softening point ASTM D-36 °C 51.2 52.5
Absolute viscosity (60 °C) ASTM D-2171 Pa s 140.5 175.2
Viscosity at 135 °C AASHTO T-316 Pa s 0.35 0.36
Ductility (25 °C, 5 cm/min) ASTM D-113 cm 139 117
Solubility in trichloroethylene ASTM D-2042 % >99 >99
Water content ASTM D-95 % <0.2 <0.2
Flash point ASTM D-92 °C 295 275
Tests on the residue after the RTFOT
Mass loss ASTM D-2872 % 0.34 0.47
Penetration of the residue after loss by heating, in % of the original penetration ASTM D-5 % 62 72

Table 2
Rheological characterization of AC 80-100.

Temperature (°C) Frequency (rad/s) d (°) G* (Pa) |G*|/sin d (kPa) |G*| sin d (kPa) Viscosity (Pa s)
AC 80-100 not aged
58 10 87 1980 1.98 1.98 212
64 10 88 776 0.78 0.78 89
70 10 89 413 0.41 0.41 39
AC 80-100 aged by RTFOT
52 10 84 9150 9.20 9.10 913
58 10 85 2698 2.71 2.69 387
64 10 88 1456 1.46 1.46 109
AC 80-100 aged by RTFOT + PAV
16 10 47 11,672,000 15959.4 8536.4 858,820
19 10 49 8,534,000 11307.6 6440.7 671,490
22 10 52 5,802,000 7362.8 4572.1 406,330

Table 3
Rheological characterization of AC 60-70.

Temperature (°C) Frequency (rad/s) d (°) G* (Pa) |G*|/sin d (kPa) |G*| sin d (kPa) Viscosity (Pa s)
AC 60-70 not aged
58 10 87 2470 2.473 2.467 245
64 10 88 1002 1.00 1.00 105
70 10 89 453 0.453 0.453 49
AC 60-70 aged by RTFOT
52 10 83 11,062 11.15 10.98 1022
58 10 85 4276 4.29 4.26 416
64 10 87 1701 1.70 1.70 138
AC 60-70 aged by RTFOT + PAV
16 10 44 14,266,000 20536.7 9910.0 967,610
19 10 45 10,193,000 14415.1 7207.6 720,080
22 10 47 6,659,000 9105.0 4870.0 488,890

After the viscosities were obtained, an Ef analysis of the AC was Ef

performed for the time period of the analysis. Ef corresponds to the
energy required for the molecules to flow from one site to another
site within the material. Ef changes with the variations in the mate-
rial viscosity, which are dependent on the temperature. When a
liquid flows, the liquid molecules require energy to move over each
other; if more energy is required, the intermolecular forces will be
greater. In this model, Eyring [18] demonstrated the feasibility of
establishing a relation between the temperature and the viscosity
using the Arrhenius Eq. (1) as follows:
Ef
ln g ¼ þ lnA ð2Þ
RT
Then, ln g was plotted versus 1/T to obtain the values of Ef/R and the
coefficient A. In this study, the activation energy increased by 0.9%
and 2.5% after one year of immersion in distilled water for AC 60-70
and AC 80-100, respectively. A potential explanation for this
increase in the stiffness and the viscosity of the binders immersed
in distilled water is that the oxygen molecules react with the
asphalt to generate an oxidation process, stiffening the binders,
and the oxidation increases the number of solid particles (increases

g ¼ AeRT ð1Þ the concentration of asphaltenes), which produces a higher resis-

where g is the material viscosity in Pa s at temperature T (K), A is a
pre-exponential factor, Ef is the flow activation energy in kJ/mole
and R is the universal gas constant [8.314 J mole1]. To facilitate
the use of the equation, the following expression was applied:
tance to flow. As a result, Ef increases.
Table 6 shows the results of the SARA test on the non-immersed
asphalt (month 0) and the asphalt immersed in distilled water for
12 months. The data show a reduction in the aromatic fractions,
which is characteristic of asphalt oxidation or aging because they
454 J.A. Hernández Noguera et al. / Construction and Building Materials 71 (2014) 451–455

Fig. 1. Evolution of the penetration with immersion time in distilled water. Fig. 4. Evolution of the absolute viscosity (60 °C) with immersion time in distilled
water.

Fig. 2. Evolution of the softening point with immersion time in distilled water. Fig. 5. Evolution of the Brookfield viscosity at 135 °C with immersion time in
distilled water.

Table 4
Rheological characterization of AC 60-70 immersed for 12 months. T and F are the
temperature and frequency, respectively.

T (°C) F (rad/s) d (°) G* (Pa) |G*|/sin d (kPa) |G*| sin d (kPa)

AC 60-70 not aged
58 10 86 2528.2 2.53 2.52
64 10 87 1237.5 1.24 1.24
70 10 88 521.6 0.52 0.52

AC 60-70 aged by RTFOT

52 10 81 12265.4 12.42 12.11
58 10 83 4597.3 4.63 4.56
64 10 86 1988.5 1.99 1.98

AC 60-70 aged by RTFOT + PAV

16 10 42 15460018.0 23104.6 10344.8
19 10 44 10666199.7 15354.6 7409.4
22 10 46 6883456.2 9569.1 4951.6
Fig. 3. Evolution of the ductility with immersion time in distilled water.

SþA
act as a dispersion path for the asphaltenes [24,25]. In both cases, IC ¼ ð3Þ
Ar þ R
the percentage of resins also decreases because they are composed
of polar aromatic compounds that are highly susceptible to oxida- Table 7 shows the ratio between the aromatics and the saturated
tion because of their structure. The colloidal index (IC) of the components (Ar/S) and the ratio between the resins and the asphalt-
asphalts, calculated using Eq. (3), increases with the immersion enes (R/A). Both ratios decrease when the asphalts are immersed in
time in distilled water and varies from 0.562 to 0.626 for the AC distilled water for 12 months. These reductions in R/A and Ar/S are
60-70 asphalt and from 0.38 to 0.519 for the AC 80-100 asphalt. characteristic of asphalt oxidation [26–29].
 J.A. Hernández Noguera et al. / Construction and Building Materials 71 (2014) 451–455 455

Table 5 aromatics fraction due to the breakage of the ring during oxidation.
Rheological characterization of AC 80-100 immersed for 12 months. T and F are the The aromatic/saturated and resins/asphaltenes ratios decreased for
temperature and frequency, respectively.
the asphalts immersed in water, which was consistent with the
AC 80-100 asphaltenes increase. The decrease in aromatic compounds and res-
T (°C) F (rad/s) d (°) G* (Pa) |G*|/sin d (kPa) |G*| sin d (kPa) ins may be responsible for the hardening observed in the asphalts.
AC 60-70 not aged
58 10 85 2223.81 2.23 2.22 References
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