coatings

Article
Freeze and Thaw Effect on Asphalt Concrete Mixtures Modified
with Natural Bentonite Clay
Mousa Ibraheem Bani Baker 1, *, Raed Mohammad Abendeh 1 and Mohammad Ali Khasawneh 2,†

1 Civil and Infrastructure Engineering Department, Faculty of Engineering and Technology,

Al-Zaytoonah University of Jordan, P.O. Box 130, Amman 11733, Jordan
2 Civil Engineering Department, Prince Mohammad Bin Fahd University, Al Azeziya,
Dhahran 34754, Saudi Arabia
* Correspondence: m.banibaker@zuj.edu.jo
† On leave from Jordan University of Science and Technology, Irbid, Jordan.

Abstract: This study aimed to investigate the effect of freeze and thaw (FT) cycles on the performance
of asphalt concrete (AC) mixtures modified by partial replacement of mineral filler of the aggregate
with natural bentonite clay (NBC) in order to reduce damage that occurs due to rapid FT cycles
within the pavement structure. After exposure to FT cycles, AC mixture stability is reduced and
becomes lower than minimum requirements, which leads to earlier damage of pavement. In order
to enhance the AC mixture’s abilities to sustain severe FT cycles, this study used NBC amounts
as a substitute for mineral filler by weight of its portion of the total aggregate: 5%, 10%, 15%, and
20%. Marshall stability, flow, and FT cycles were tested, and interior damage degree was assessed
by a nondestructive test called ultrasonic pulse velocity (UPV). The results revealed the viability
of combining NBC with asphalt mixtures for the purpose of improving the mixtures’ properties,
particularly in environments where asphalt pavement is exposed to alternating FT cycles. The results
also revealed that replacement of filler with NBC by 5% in AC mixtures reduced the damage caused
Citation: Bani Baker, M.I.; over 8 continuous weeks of rapid FT cycles by 13%, which, in future applications, would reduce
Abendeh, R.M.; Khasawneh, M.A. maintenance cost and prolong the pavement’s service life.
Freeze and Thaw Effect on Asphalt
Concrete Mixtures Modified with
Keywords: freeze thaw; bentonite clay; mineral filler; aggregate; pavement; asphalt concrete mixtures;
Natural Bentonite Clay. Coatings 2022,
ultrasonic pulse velocity; damage index
12, 1664. https://doi.org/10.3390/
coatings12111664

Academic Editors: Nhu H.T. Nguyen

and Mingjing Fang 1. Introduction
Received: 25 September 2022 Asphalt pavements can withstand substantial loads and environmental conditions for
Accepted: 28 October 2022 a reasonable time [1]. Various forms of admixtures have been used to prolong the service-
Published: 2 November 2022 ability life of pavements by alleviating temperature effect and cracking of asphalt concrete
(AC) mixtures [2,3]. Numerous studies have shown that in this use, fiber, hydrated lime,
Publisher’s Note: MDPI stays neutral
waste plastics, and traditional polymers could develop properties of AC [4,5]. However,
with regard to jurisdictional claims in
high-temperature stability and low-temperature cracking-resistance requirements could not
published maps and institutional affil-
iations.
be satisfied for many asphalt and improved AC mixes [6]. Therefore, new admixtures were
investigated in order to improve the performance of AC mixtures: for example, nano-clay.
These improved mixes were found to show better rutting resistance than traditional AC
pavements (without additives), according to AASHTO T283 [7]. The high surface area of
Copyright: © 2022 by the authors. nano-clay (700–800 m2 /g) is due to the separation of clay discs, which creates an interface
Licensee MDPI, Basel, Switzerland. between nano-clay and asphalt. Nano-particles, nano-silica, nano-tubes, and bentonite
This article is an open access article clay were suggested to be added to the AC mix to raise the viscosity of binders and to
distributed under the terms and enhance rutting and fatigue resistance [8,9]. Fillers were principally categorized by capacity
conditions of the Creative Commons to stiffen and thicken asphalt film [10]. These clay materials can commonly be utilized in
Attribution (CC BY) license (https:// road-construction projects as a substitute for a natural aggregate of hot mix asphalt (HMA)
creativecommons.org/licenses/by/ production as long as their unwanted features are reduced [11].
4.0/).

Coatings 2022, 12, 1664. https://doi.org/10.3390/coatings12111664 https://www.mdpi.com/journal/coatings

Coatings 2022, 12, 1664 2 of 14

AC mixtures are affected by two major forms of loading: mechanical loading, particu-
larly because of hefty trucks; and climate, due to temperature, moisture, and freezing and
thawing (FT) cycles. An expansion of 9% occurs when water turns to ice under freezing con-
ditions. Asphalt pavements deteriorate over time as a result of environmental effects and
heavy traffic loading on paving elements [12]. Rutting, fatigue cracking, low-temperature
cracking, and moisture-induced damage (stripping) are the main distresses accountable for
degradation of AC, subsequently leading to its failure [13,14]. Freezing and thawing cycles
cause damage to the binder, which can be seen in reduction of stiffness as freezing and
thawing intensity increases. The bond between asphalt and aggregate weakens when water
infiltrates the pavement, resulting in a reduction in adhesion, normally called “stripping,”
that is the key degradation mechanism throughout FT cycles [15–18].
During FT cycles, ambient temperature frequently varies, as does pavement wear from
frequent thermal stresses and moisture impacts. The resilient modulus and compressive
strength of AC mix drop when AC is exposed to FT cycles [19].
If water in the spaces of pavement solidifies to ice in a cold environment, the mix
will be exposed to growing stress; however, at warmer temperatures (during and after the
thawing process), the AC structure will detach [20–24]. This expansion force results in
micro-damage to the pavement material. Throughout the melting cycles, additional water
fills the air voids. Therefore, the inner arrangement of the mixture is seriously damaged
by FT in cold areas [25]. Marshall stability is reduced when FT cycles are increased [26].
FT cycles escalate the sizes of existing pores and cause the occurrence of new pores in AC
pavements [27].
Natural clays are not currently used as AC admixtures; in fact, aggregate specifications
recommend avoiding aggregates with excessive clay amounts. This is because clay gener-
ates a mineral that covers the aggregate surface, causing the hot asphalt to attach to the clay
and not to the aggregate underneath. The asphalt is then vulnerable to moisture damage
because water will relocate the clay particles and then strip the binder from the aggregate
surface. However, addition of a specific type of clay, namely natural bentonite clay (NBC),
as a replacement of the AC mix’s mineral filler in a controlled amount will overcome the
negative aspects of clay additives in AC mixtures, leading to improvement of AC mixture
specifications. In fact, fractional replacement of mineral filler with NBC at 15% fulfills
design requirements for medium traffic [28]. FT cycles on pavement result in reduction
of the pavement’s stability; consequently, the pavement will be damaged and need con-
siderable maintenance or replacement. This damage and maintenance are associated with
costs that lead to direct burdens on municipalities, governments, and private businesses’
toll-highway budgets. Constructing a highway is very expensive and might cost from 6 to
12 million euros per kilometer in Europe (depending on terrain and country), while in the
United States of America, a major freeway of four lanes may cost over 40 million dollars
per kilometer. Therefore, increasing attention is needed to study and mitigate the effect
of FT cycles on pavements, which might cause billions of dollars in losses and human
fatalities due to road accidents. In this study, performance of improved AC mixtures after
partial replacement of the aggregate’s mineral filler with NBC subjected to the FT cycle
effect was investigated in order to introduce a practical solution for damaged pavements in
cold regions subjected to severe FT cycles. The incorporation of abundantly available and
economically affordable NBC in AC could lead to both sustainable pavement construction
and environmental preservation. It is therefore necessary to expand existing research on
asphalt and AC modification in order to inspect the effect of asphalt modification with
NBC on physical, rheological, and mechanical properties of asphalt pavements, especially
under FT conditions.

2. Mixtures
2.1. Aggregate
Medium-density crushed limestone aggregate from Amman-Jordan was used in this
study because that type of crushed limestone aggregate is abundant in Jordan, with a
 Coatings 2022, 12, x FOR PEER REVIEW 3 of 14

2. Mixtures
Coatings 2022, 12, 1664 2.1. Aggregate 3 of 14

Medium-density crushed limestone aggregate from Amman-Jordan was used in this

study because that type of crushed limestone aggregate is abundant in Jordan, with a rea-
reasonable
sonable costcost
for for
road road construction.
construction. JordanJordan governmental
governmental data
data for for Public
Public WorksWorksand Hous- and
Housing Gradation
ing Gradation 20102010 [29] was
[29] was usedused
as a as a reference
reference standard
standard in this
in this research
research to prepare
to prepare the
the aggregate as shown in Figure 1, which indicates that 70% of the total
aggregate as shown in Figure 1, which indicates that 70% of the total aggregate was coarse aggregate was
coarse aggregate,
aggregate, 25% was 25%finewasaggregate,
fine aggregate,
and 5%and 5%the
was wascontribution
the contribution
of theofmineral
the mineralfiller.filler.
Our
Our target was to replace 5% of the weight of the mineral
target was to replace 5% of the weight of the mineral filler with NBC. filler with NBC.
Table
Table11demonstrates
demonstratesthe thetested
testedcompositions
compositions of of
aggregate
aggregate gradation
gradationwithwithandandwithout
with-
bentonite, whilewhile
out bentonite, TableTable
2 shows the properties
2 shows of theofaggregates
the properties used in
the aggregates thisinstudy
used [28]. XRF
this study [28].
was utilized to obtain the chemical compositions of natural aggregate
XRF was utilized to obtain the chemical compositions of natural aggregate and filler. Theand filler. The XRF
analysis showed
XRF analysis that CaO
showed thatwasCaO thewas
highest oxide inoxide
the highest the limestone aggregate,
in the limestone with 53.52%,
aggregate, with
followed by SiO 2 (3.45%), Fe 2 O 3 (2.12%), and MgO
53.52%, followed by SiO2 (3.45%), Fe2O3 (2.12%), and MgO (2.05%).(2.05%).

Lower Limit Upper Limit

100

80
Percent Passing

60

40

20

0
100 10 1 0.1 0.01
Sieve Size (mm)

Figure1.1.Aggregate
Figure Aggregategradation.
gradation.

Table1.1.Amounts
Table Amountsofofaggregate,
aggregate,filler,
filler,and
andNBC.
NBC.

NBC (%) NBC

NBC (%) (g)
NBC (g) Filler (g) Coarse
Filler (g) Aggregate(g)(g) Fine
Coarse Aggregate Aggregate(g)(g) Total
Fine Aggregate AC(g)
Total AC (g)
00 0
0 55
55 770
770 275
275 1100
1100
5 2.75 52.25 770 275 1100
5 2.75 52.25 770 275 1100
10 5.5 49.5 770 275 1100
10 5.5 49.5 770 275 1100
15 8.25 46.75 770 275 1100
15 8.25 46.75 770 275 1100
20 11 44 770 275 1100
20 11 44 770 275 1100
Table 2. Aggregate physical properties.
Table 2. Aggregate physical
ASTMproperties. Absorption (%) =
Aggregate (Gsb) = A/(B–C) (Gsa) = A/(A–C)
Designation
ASTM (B–A)100/A(%)
Absorption
Aggregate
Coarse C127 (G sb ) = A/(B–C)
2.501 (G2.522
sa ) = A/(A–C) 4.50
Designation = (B–A)100/A
Fine
Coarse C128C127 2.4702.501 2.485 2.522 7.01
4.50
Filler
Fine
C128C128 2.5152.470 2.534 2.485
-----
7.01
Gsb = bulk specific gravity; Gsa = apparent specific gravity; A = mass of oven-dried aggregate in air
(g); B =Filler C128 dry (SSD) aggregate
mass of saturated surface 2.515 in air (g); C2.534
= mass of submerged —–aggregate
Gin = bulk (g).
sb water specific gravity; Gsa = apparent specific gravity; A = mass of oven-dried aggregate in air (g); B = mass
of saturated surface dry (SSD) aggregate in air (g); C = mass of submerged aggregate in water (g).

2.2. Bitumen
2.2. Bitumen
Bitumen grade 85/100 from the Jordan Petrol Corporation was used in this study,
Bitumen grade 85/100 from the Jordan Petrol Corporation was used in this study, with
with 85/100 (0.1 mm) penetration at 25 °C, 100 cm ductility at 25 °C, 1.01 specific gravity
85/100 (0.1 mm) penetration at 25 ◦ C, 100 cm ductility at 25 ◦ C, 1.01 specific gravity at
25 ◦ C, a 49 ◦ C softening point, a 235 ◦ C flash point, a 249 ◦ C fire point, and 99% solubility
in trichloroethylene.
 Coatings 2022, 12, x FOR PEER REVIEW 4 of 14

Coatings 2022, 12, 1664 4 of 14

at 25 °C, a 49 °C softening point, a 235 °C flash point, a 249 °C fire point, and 99% solubility
in trichloroethylene.

2.3.
2.3.Bentonite
Bentonite
NBC
NBC passing
passing US USsieve
sieveno.no. 200
200 from
from Al-Azraq-Jordan
Al-Azraq-Jordan was was used
used inin this
this study,
study,with
with
2.62 g/cm33 specific
2.62g/cm specific gravity,
gravity, 8%8% water
water content,
content,420420mm22/g surface area, and 190% absorption.
/g surface absorption.
The
Thechemical
chemicalcomposition
composition of of
NBCNBC is shown in Table
is shown 3. The
in Table 3. mineral composition
The mineral of theof
composition NBC
the
was
NBCobtained by exposure
was obtained of the of
by exposure clay
thetoclay
XRD to analysis. Clay size
XRD analysis. Clayfraction was separated
size fraction was sepa-
using
rated Atterberg’s procedure.
using Atterberg’s For clay
procedure. Forpatterns, resultsresults
clay patterns, were introduced as peakaspositions
were introduced peak po-
at 2θ and intensity in the form of counts as presented in Figure
sitions at 2θ and intensity in the form of counts as presented in Figure 2 [28],2 [28], which alsowhich
indicates
also
that the NBC
indicates thatused in this
the NBC study
used wasstudy
in this not pure,
was comprising smectite-montmorollinite
not pure, comprising smectite-montmorol-and
amounts
linite andofamounts
illite, kaolinite,
of illite,quartz, dolomite,
kaolinite, quartz, and calcite.and
dolomite, NBC was added
calcite. NBC was to AC mixtures
added to AC
in small doses
mixtures to partially
in small doses toreplace
partiallymineral filler
replace in thefiller
mineral aggregate
in the gradation
aggregateand reduceand
gradation its
swelling behavior.
reduce its swelling behavior.

Figure2.2.Representative
Figure RepresentativeXRD
XRDpatterns
patternsof
oforiented
orientedsamples
samplesfor
forAl-Azraq
Al-AzraqNBC.
NBC.

Table3.3.Chemical
Table Chemicalanalysis
analysisofofNBC
NBCby
byXRF.
XRF.

Oxide SiO2 Al2O3 Fe2O3 MgO CaO Na2O K2O TiO2 MnO LOI
Oxide SiO2 Al2 O3 Fe2 O3 MgO CaO Na2 O K2 O TiO2 MnO LOI
Percent 53.11 16.84 9.15 4.40 0.45 0.91 2.32 1.70 0.05 10.23
Percent 53.11 16.84 9.15 4.40 0.45 0.91 2.32 1.70 0.05 10.23

3. Test Procedure
3. Test Procedure
3.1. Marshall Test
3.1. Marshall Test
Following the well-known and well-documented Marshall test procedure for as-
Following the well-known and well-documented Marshall test procedure for asphalt-
phalt-mixture stability and flow (ASTM D1559) [30] and air-void and bulk density (ASTM
mixture stability and flow (ASTM D1559) [30] and air-void and bulk density (ASTM
D2726-96) [31] enabled the determination of optimum asphalt content (OAC) that satisfied
D2726-96) [31] enabled the determination of optimum asphalt content (OAC) that satisfied
design requirements under medium traffic conditions. Accordingly, OAC was found to
design requirements under medium traffic conditions. Accordingly, OAC was found to be
be 5.5% by weight of total asphalt mixture, thus used in sample production. NBC was
5.5% by weight of total asphalt mixture, thus used in sample production. NBC was used
used in this study because it is available in Jordan and other countries in the region, mak-
in this study because it is available in Jordan and other countries in the region, making it
ing it inexpensive
inexpensive to substitute
to substitute mineralmineral filleraggregate
filler of the of the aggregate
in the ACinmix
theby
AC mix by
varied varied
amounts
amounts of weight: initially 0% for control, then 5%, 10%, 15%, and 20%. Added
of weight: initially 0% for control, then 5%, 10%, 15%, and 20%. Added NBC was a partial NBC was
substitution of filler; if its maximum case (20% of mineral filler) did not exceed 1% of the
total aggregate in the asphalt mixture, then the increase in OAC was negligible. Therefore,
Coatings 2022, 12, x FOR PEER REVIEW 5 of 14

a partial substitution of filler; if its maximum case (20% of mineral filler) did not exceed
Coatings 2022, 12, 1664 5 of 14
1% of the total aggregate in the asphalt mixture, then the increase in OAC was negligible.
Therefore, for the practicality of the application, OAC was fixed at 5.5% for all samples
(all test results presented are from an average of three samples for each asphalt mixture).
for the practicality of the application, OAC was fixed at 5.5% for all samples (all test results
Figure 3e shows NBC variations with original and retained stability (RS), which were
presented are from an average of three samples for each asphalt mixture).
above the minimum requirement. RS was evaluated after submersion of the specimens in
Figure 3e shows NBC variations with original and retained stability (RS), which were
water for 24 h. The submerging procedure comprised immersing AC specimens in a water
above the minimum requirement. RS was evaluated after submersion of the specimens in
bath
waterat for
25 24
°Ch.for
The24submerging
h to simulate a harshcomprised
procedure environment; after that,
immersing specimensinwere
AC specimens inun-
a water
dated in a water
◦ bath at 60 °C for 30 min. Stability of modified mixtures
bath at 25 C for 24 h to simulate a harsh environment; after that, specimens were inundated decreased with
increasing NBCatcontent
in a water bath over
60 ◦ C for 15%,Stability
30 min. which ofis modified
consistent with the
mixtures trend ofwith
decreased density (Figure
increasing
3a) and VFA (Figure 3d) for the modified AC mixtures with the lowest
NBC content over 15%, which is consistent with the trend of density (Figure 3a) and VFAair voids and VMA
(Figure
(Figure3b,c), and
3d) for thewhich
modified might
AC be a result
mixtures of reduction
with in adhesion
the lowest air voids andof bitumen
VMA to3b,c),
(Figure the ag-
gregate
and whichand might
separation
be a of the of
result aggregate
reductionin in
theadhesion
specimen. The mixing
of bitumen procedure
to the aggregate followed
and
inseparation
preparingofthe thelaboratory
aggregate in ACthespecimens
specimen. wasThe exactly
mixing procedure followed
as is outlined in preparing
in a previous study
the
[28]. laboratory AC specimens was exactly as is outlined in a previous study [28].

2.190 6.00
Density (g/cm3)

Air Void (%)

2.180
4.00
2.170
2.00
2.160
2.150 0.00
0 5 10 15 20 0 5 10 15 20
% Bentonite (%) Bentonite

(a) (b)
17.50 80.00
78.00
17.00
VMA (%)

VFA (%)

76.00
16.50 74.00
72.00
16.00
70.00
15.50 68.00
0 5 10 15 20 0 5 10 15 20
(%) Bentonite (%) Bentonite

(c) (d)
12
Original Stability
10 Retained Stability

8 Poly. (Original Stability)

Stability (kN)

6 Poly. (Retained Stability)

0
0 5 10 15 20 25 30
% Bentonite
(e)
Figure
Figure3.3.Bentonite
Bentonitevariation
variation with
with (a) density,(b)
(a) density, (b)air
airvoid,
void,(c)(c)VMA,
VMA,(d)(d) VFA,
VFA, and
and (e)(e) original
original andand
retained stability (the green dotted line represents the minimum requirement for stability).
retained stability (the green dotted line represents the minimum requirement for stability).
 ASTM C666-Procedure A [32,33]. This procedure was carefully evaluated in t
termination of FT resistance of asphalt mixtures; the testing procedure was dee
ising and suitable to be used for the purpose of asphalt-mixture FT resistance
Coatings 2022, 12, 1664
[34]. 6 of 14
In order to conduct FT cycles on AC specimens, each specimen was pr
plastic zip-lock with the addition of 10 ± 0.5 mL of water before the FT proces
loss
3.2. FTof moisture. Next, specimens were removed from the bags and placed in
Procedure
to be subjected
Cylindrical AC to a designated
specimens number
were exposed of FT cycles
to repeated at in
FT cycles a accordance
temperature withof −18 a
ASTM C666-Procedure A
repeated cycles of 4 h each.[32,33]. This procedure was carefully evaluated in terms of deter-
mination of FT resistance of asphalt mixtures; the testing procedure was deemed promising
Specimens
and suitable to be usedwere removed
for the purpose of from the chamber
asphalt-mixture in a thawed
FT resistance condition
simulation [34]. at the
week, thentodried
In order conductusing a towel
FT cycles on ACand testedeach
specimens, in addition
specimen was for protected
damageinusing a an
plastic zip-lock with the addition of 10 ± 0.5 mL of water before the
velocity (UPV) test to estimate average weight loss of AC mixtures by measu FT process to prevent
loss of moisture. Next, specimens were removed from the bags and placed in a chamber
erage weight of three specimens for each AC mixture after FT cycles: satura
to be subjected to a designated number of FT cycles at a temperature of −18 and 4 ◦ C for
dry (SSD)
repeated compared
cycles of 4 h each. to weight of the control sample before its subjection to t
Next, another
Specimens FTremoved
were cycle wasfromcommenced
the chamber inby placing
a thawed specimens
condition back
at the end of into
each the ch
week, then dried using a towel and tested in addition for damage
which the process was repeated for a specified number of weeks. Finally, specusing an ultra pulse
velocity (UPV) test to estimate average weight loss of AC mixtures by measuring the
tested for Marshall stability and flow at the end of week 8.
average weight of three specimens for each AC mixture after FT cycles: saturated surface
dry (SSD) compared to weight of the control sample before its subjection to the FT cycle.
3.3. Ultrasonic
Next, Pulse
another FT cycle wasVelocity (UPV)
commenced Measurement
by placing specimens back into the chamber, after
which the process was repeated for a specified number of weeks. Finally, specimens were
Ultra pulse velocity (UPV) equipment was used to evaluate the damage
tested for Marshall stability and flow at the end of week 8.
various AC mixtures under varied FT cycles. Figure 4 shows the experimen
3.3.
theUltrasonic Pulse Velocity (UPV)
UPV measurement Measurement
performed in the laboratory for testing AC specimens.
Ultra
pulse was pulse velocity (UPV)
converted intoequipment
mechanical was vibration
used to evaluate the damage
through induced in
a transducer attached
various AC mixtures under varied FT cycles. Figure 4 shows the experimental setup of the
facemeasurement
UPV of the asphalt concrete
performed sample. for
in the laboratory A receiving transducer
testing AC specimens. was placed
The electric pulse on th
face
was of the sample.
converted The receiving
into mechanical transducer,
vibration through which
a transducer received
attached propagating
to one end face of wav
the
pled to an interior timer in the equipment, which instantaneouslyface
asphalt concrete sample. A receiving transducer was placed on the other end of
showed the
the sample. The receiving transducer, which received propagating waves, was coupled to
of the wave [24]. The wave speed was calculated by dividing the length of th
an interior timer in the equipment, which instantaneously showed the travel time of the
by the
wave [24].travel
The wavetime. It was
speed important
was calculated to guarantee
by dividing thatof athecontinuous
the length specimen by pressure
the w
steadily to the transducer to ensure enough contact between transducers and s
travel time. It was important to guarantee that a continuous pressure was applied steadily
totothe transducer
deliver to ensuredata.
accurate enough Incontact between
general, the transducers
higher the and samples and
velocity was, to deliver
the better th
accurate data. In general, the higher the velocity was, the better the quality of the material
theinmaterial
was was in
terms of density, terms of
uniformity, density, uniformity,
homogeneity, and continuity, homogeneity, and continui
whereas slower velocities
slower
may have velocities
indicated ACmay withhave
severalindicated ACcavities.
cracks and/or with several cracks and/or cavities.

Figure
Figure 4. Ultrasonic
4. Ultrasonic pulse velocity
pulse velocity measurement.
measurement.

Damage indices (DI) were then found and used for investigation of th
modification of asphalt concrete mixtures with NBC on resistance to freezing a
cycles. DI in terms of UPV was calculated using the following equation [24]:
Coatings 2022, 12, 1664 7 of 14

Damage indices (DI) were then found and used for investigation of the impact of
modification of asphalt concrete mixtures with NBC on resistance to freezing and thawing
cycles. DI in terms of UPV was calculated using the following equation [24]:
" #2
UPVdam
DIUPV = 1 − ◦ (1)
UPV

where UPV◦ is initial ultrasonic pulse velocity and UPVdam is ultrasonic pulse velocity after
a certain number of FT cycles [24]. The relationship between DIUPV and additive (NBC)
variation, along with various FT cycles, was inspected.

4. Results and Discussions

Based on results obtained by several researchers, bentonite clay could be considered
a technically feasible choice as a substitute material to replace natural filler in hot mix
asphalt. Considering the global need to ensure well-performing road infrastructures while
using environmentally sound construction technologies, the use of bentonite clays as road
pavement stabilizers could be of interest to several road investors [35]. Heavy vehicle loads
and seasonal temperature changes can impact the rheological and mechanical properties
of AC; pavements designed and constructed to withstand medium-heavy traffic require
engineered pavement mixtures [36]. Therefore, this research was focused on improving
AC mixtures that are used for flexible pavement purposes in roads, highways, and other
important AC paving projects in cold regions that undergo high seasonal temperature
variations. The main objective in this research was to reduce the damage that occurs within
the AC pavement structure in order to minimize the maintenance and management cost of
these structures.
The findings of this research revealed that stability of modified AC mixtures rose with
increased NBC content. When an improved AC mix was amended by 15% NBC compared
to the control sample, a 26% enhancement was recorded. Stability reduced when NBC was
increased over 15%, which is in line with the tendency of density in the improved AC mix
with NBC. This could be a result of a decrease in adhesion of bitumen to aggregate and
detachment of the aggregate in the AC sample.
Figures 5 and 6 show average weight loss and average corrected stability of AC
mixtures with different NBC contents after 8 weeks of FT cycles. Both average weight loss
and corrected stability rose with the increase of NBC and touched their highest values
when NBC was 10%; that corresponded with 6.6% weight loss and 7 kN corrected stability,
respectively. Moreover, Figure 6 shows that the stability for the unmodified specimen with
0% NBC dropped drastically after 8 weeks of FT cycles, reaching 4.1 kN, which is below
the minimum requirement, as indicated by the dotted green line. However, for 5%, 10%,
and 15% modification of NBC, stability results were above the minimum requirement, at
6.1 kN and 7 kN, respectively. At 15% substitution of filler with NBC, the value of corrected
stability met minimum requirements for medium traffic conditions after 8 continuous
weeks of FT cycles. Increasing the NBC to above 15% resulted in a reduction in asphalt
stability, which can be attributed to the ability of NBC to absorb more moisture, resulting
in loss of adhesion between asphalt and aggregate and therefore causing reduction of
pavement stability.
Coatings 2022,12,
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7.0
7.0
6.0
6.0

(%)
loss(%)
5.0
5.0

weightloss
4.0
Averageweight
4.0
3.0
3.0
Average

2.0
2.0
1.0
1.0
0.0
0.0
0%
0% 5%
5% 10%
10% 15%
15% 20%
20% 25%
25%
Bentonite content
Bentonite content (%)
(%)

Figure5.5.
Figure
Figure 5.Average
Averageweight
Average weightloss
weight lossofof
loss ofACACwith
AC withbentonite
with bentonitevariation
bentonite variationafter
variation after888weeks
after weeksofof
weeks ofFT
FTcycles.
FT cycles.
cycles.

14
14

12
12

10
10
(kN)
Stability(kN)

88 Stability at
at 00 FT
FT cycle
cycle
Stability
Stability

(kN)
(kN)
66
Stability after
Stability after 88 weeks
weeks
of FT cycles (kN)
of FT cycles (kN)
44

22

00
00 55 10
10 15
15 20
20 25
25
Bentonite content
Bentonite content (%)
(%)

Figure 6.
Figure 6. Average
Average corrected
corrected stability
stability (kN)
(kN) vs
vs bentonite
bentonite content
content variation
variation with
with FT
FT cycles.
cycles. The
The green
green
Figure 6. Average corrected stability (kN) vs bentonite content variation with FT cycles. The green
dotted line
dotted line represents
represents the
the minimum
minimum requirement
requirement for
for stability.
stability.
dotted line represents the minimum requirement for stability.
Whenwater
When
When waterentered
water entered
entered thethe
the
AC, AC,
AC, the
thethe
bond bond
bond between
between
between bitumenbitumen
bitumen and
and and aggregate
aggregate
aggregate decreased
decreased
decreased and
and
there there
and there was
was awas a reduction
a reduction
reduction in adhesion,
in adhesion,
in adhesion, frequently
frequently
frequently termed termed
termed as “stripping.”
as “stripping.”
as “stripping.” FT cycles
FT cycles
FT cycles caused
causedcaused
more
more separation
more separation
separation and anand and
increasean increase
an increase
in air void in air
in air void in
void
content content
content
asphalt inpavement.
in asphalt pavement.
asphalt pavement. This,resulted
This,
This, in turn, in turn,
in turn,
resulted
in different
resulted in different
in asphalt
different asphalt
concrete concrete
asphaltdistresses, distresses, such
such as cracking,
concrete distresses, as cracking,
such as flushing, flushing,
cracking,raveling,
flushing,and raveling, and
bleeding.
raveling, and
bleeding. Replacing
Replacing
bleeding. Replacing
a portion of aa portion
portion
the fillerof ofofthe
the filler
thefiller
AC of of
mixthewith
the AC NBC
AC mix with
mix with NBC
in a NBC in aa controlled,
controlled,
in controlled, limited
limited amount
limited
amount
resulted resulted
in filling in
of filling
the voids of the
when voids
the when the
bentonite bentonite
expanded
amount resulted in filling of the voids when the bentonite expanded due to increase in expanded
due to due
increase toinincrease
moisture in
moisture
and
moisture and
the effect
and of the
theFTeffect of
cycles,
effect FT
of FT cycles,
which
cycles, which
resulted
whichin resulted in
an increase
resulted an
in an in increase in AC
AC stability.
increase stability.
Causes such
in AC stability. Causes
Causesas
such as
frequent
such as temperature
frequent temperature
frequent temperature
variation and variation
FT cycles
variation andinFT
and FT cycles
winter
cycles also in produced
in winter also
winter also produced
stiffness
produced stiffness
reduction
stiffnessof
reductionlayers,
pavement
reduction of pavement
of pavement
particularlylayers,
layers, particularly
theparticularly
surface layer thethat
the surface
expedited
surface layer longitudinal
layer that expedited
that expedited longitudinal
andlongitudinal
transverse
and transverse
cracks
and transverse cracks of
of the top-down
cracks oftype.
the top-down
the top-down type. It
It also expedited
type. It also
also expedited
theexpedited
load-associatedthe load-associated
the load-associated
fatigue damage fatigue
by
fatigue
damage
worsening by worsening
the horizontal the horizontal
tensile stresses tensile
at the stresses
bottom at
of the bottom
asphalt
damage by worsening the horizontal tensile stresses at the bottom of the asphalt layer. In of the
layer. asphalt
In fact, layer.
cracking In
fact,
and cracking
stripping and
increased stripping
with increased
the influence with
of the
FT influence
cycles. of FT
Environmental
fact, cracking and stripping increased with the influence of FT cycles. Environmental cycles. Environmental
stresses are of key
stresses are
importance
stresses are inof affecting
of key importance
key importance
pavement in affecting
in affecting pavement
construction.
pavementThese construction. These
stresses canThese
construction. stresses can
substantially
stresses can sub-
change
sub-
stantially
the stiffness
stantially change the
of asphalt
change stiffness
pavement.
the stiffness of asphalt pavement.
High temperatures
of asphalt pavement. High Highcould temperatures could
cause the viscoelastic
temperatures cause
could causeand the
the
viscoelastic and
thermoplastic
viscoelastic and thermoplastic
asphalt asphalt
to behaveasphalt
thermoplastic to behave
behave
like a viscous
to likewhich
fluid,
like aa viscous
viscous fluid,
mayfluid, which
lead which
to mayOn
rutting.
may lead
lead theto
to
Coatings 2022, 12, x FOR PEER REVIEW 9 of 14
Coatings 2022, 12, x FOR PEER REVIEW 9 of 14

Coatings 2022, 12, 1664 9 of 14

rutting.
rutting. On
On thethe other
other hand,
hand, low low temperatures
temperatures (especially
(especially temperatures
temperatures below below thethe freezing
freezing
point)
point) cause asphalt
cause lowasphalt to act more like
to act more(especially an elastic
like an elastic solid that is
solid that below more
is morethe susceptible
susceptible to low tem-
to lowcause
tem-
other hand,
perature cracking. temperatures
Therefore, loss of temperatures
durability of asphalt mixtures freezing
under point)
freezing and
perature cracking.
asphalt tocycles
act more Therefore,
like an elastic loss of
solid durability
that is more of asphalt
susceptible to mixtures under
low temperature freezing and
cracking.
thawing
thawing cycles deserves
deserves research
research attention.
attention. Consequently,
Consequently, stress
stress and
and deformation
deformation in
in
Therefore,
HMA due loss
to of durability
variant thermal of asphalt
expansion mixtures
and under freezing
contraction can and thawing
cause cyclesof
generation deserves
cracks
HMA due to variant thermal expansion and contraction can
research attention. Consequently, stress and deformation in HMA due to variant thermal cause generation of cracks
[17].
[17].
expansion and contraction can cause generation of cracks [17].
Figure
Figure 7 shows that flow values decreased with an increase of
of NBC content in
in mod-
Figure 77 shows
showsthatthatflow
flowvalues
valuesdecreased
decreased with
with anan increase
increase of NBC NBC content
content mod-
in modified
ified
ified mixtures
mixtures when
when subjected
subjected to
to 88 weeks
weeks of
of freezing
freezing and
and thawing.
thawing. The
The flow
flow at
at 5%
5% and
and
mixtures when subjected to 8 weeks of freezing and thawing. The flow at 5% and 10% NBC
10%
10% NBC
NBC reached
reached 6.2
6.2 and
and 5.5
5.5 mm,
mm, respectively.
respectively. Reduction
Reduction in
in flow
flow was
was insignificant
insignificant with
with
reached 6.2 and 5.5 mm, respectively. Reduction in flow was insignificant with an increase
an
an increase
increase of
of NBC.
NBC. Without the FT effect,
effect, flow increased with
withofan increase of NBC, from
of NBC. Without the Without
FT effect,the flowFTincreased flowwithincreased
an increase an increase
NBC, from of3.7NBC,
mm at from
0%
3.7
3.7 mm
mm at
at 0%
0% NBC
NBC to
to 4.45
4.45 mm
mm at
at 10%
10% NBC;
NBC; after
after that,
that, a
a reduction
reduction in
in flow
flow was
was recorded
recorded
NBC to 4.45 mm at 10% NBC; after that, a reduction in flow was recorded with an NBC
with
with an
an NBC
NBC increase. The test
test results showed that 5%
5% and 15%
15% NBC contents met
met asphalt
increase. The increase.
test resultsTheshowed results
that 5%showed
and 15% thatNBC and
contents NBC contentsrequirements
met asphalt asphalt
requirements
requirements concerning
concerning flow
flowforand
and stability
stability for medium
for medium traffic
traffic conditions
conditions before and
and after
concerning flow and stability medium traffic conditions before and afterbefore after
being subjected
being
being subjected
subjected to to FT
FT cycles.
cycles.
to FT cycles.

Figure
Figure 7.
7. Flow
Flow with
with bentonite
bentonite clay
clay variation
variation at different FT cycles.
at different FT cycles.

Figures
Figures 88 and
and 99 represent
represent average
represent average velocity
average velocity UPV
velocity UPV (km/s)
(km/s) and
UPV (km/s) and the
and the damage
damage index
index for
for
asphalt
asphalt mixtures
mixtures with
with various
various bentonite
bentonite clay
clay contents
contents when
when subjected
subjected to
to FT
FT cycles.
cycles.
asphalt mixtures with various bentonite clay contents when subjected to FT cycles.

Average
Figure 8. Average
Figure content variation (%).
Figure 8.
8. Average velocity
velocity versus
versus FT
FT cycles
cycles for
for AC
AC with
with bentonite
bentonite content variation (%).
Coatings 2022,
Coatings 2022, 12,
12, 1664
x FOR PEER REVIEW 10
10 of 14
of 14

Figure 9. Damage index versus FT cycles

Figure 9. cycles for
for AC
AC with
with bentonite
bentonite content
content variation
variation (%).
(%).

The resultsdisplayed
The results displayedthat thatthethe velocity
velocity of nondestructive
of nondestructive pulses
pulses throughthrough
asphalt asphalt
spec-
specimens increased by 7.85% at 5% NBC content before application
imens increased by 7.85% at 5% NBC content before application of the FT effect. However, of the FT effect.
However,
velocity was velocity
reducedwaswhen
reduced when specimens
specimens were subjected
were subjected to FT For
to FT cycles. cycles. For instance,
instance, after 8
after 8 weeks of FT cycles, velocity was reduced by 30% for control/unmodified
weeks of FT cycles, velocity was reduced by 30% for control/unmodified specimens and specimens
and
25% 25% for modified
for modified mixturesmixtures
with 5% with
NBC. 5%In NBC.
spiteIn of spite of that,
that, when when specimens
specimens were subjectedwere
subjected to 8 weeks of FT effect, the velocity of 5% modified AC
to 8 weeks of FT effect, the velocity of 5% modified AC mixtures was 15% higher than that mixtures was 15% higher
than that ofmixtures.
of control control mixtures.
Likewise,Likewise,
the damage the index
damage forindex for 5% modified
5% modified mixturesmixtures after
after 8 weeks
8 weeks of FT cycles was 13% less than that of control samples, indicating that less damage
of FT cycles was 13% less than that of control samples, indicating that less damage oc-
occurred when bentonite clay was used in asphalt-mixture modification. The action of pore
curred when bentonite clay was used in asphalt-mixture modification. The action of pore
pressure due to FT cycles caused the damage and fracturing of microcracks; then small
pressure due to FT cycles caused the damage and fracturing of microcracks; then small
cracks were produced, leading to the appearance of large cracks [37].
cracks were produced, leading to the appearance of large cracks [37].
Interestingly, weight-loss values after 8 weeks of FT cycles indicated that the least
Interestingly, weight-loss values after 8 weeks of FT cycles indicated that the least
loss was in mixtures modified by 5% bentonite, with 3.3% loss as compared to 4.5%, 6.5%,
loss was in mixtures modified by 5% bentonite, with 3.3% loss as compared to 4.5%, 6.5%,
and 4.7% loss for mixtures modified with 7%, 10%, and 15% NBC, respectively, illustrated
and 4.7% loss for mixtures modified with 7%, 10%, and 15% NBC, respectively, illustrated
by Figure 5. That is why chosen optimum bentonite content was 5%. Moreover, 5%
by Figure 5. That is why chosen optimum bentonite content was 5%. Moreover, 5% NBC
NBC replacement of the mineral filler is a very low amount, as mineral filler forms only
replacement of the mineral filler is a very low amount, as mineral filler forms only 55 g
55 g out of 1100 g of the total aggregate; that means the replacement was calculated as
out of 1100 g of the total aggregate; that means the replacement was calculated as 0.05 ×
0.05 × 55 = 2.75 g NBC and 52.25 g mineral filler to be added to 770 g coarse aggregate
55=2.75
and 275 gfineNBC and 52.25This
aggregate. g mineral
amountfiller to be(0.25%
of NBC addedoftototal
770 g coarse aggregate
aggregate) is very low andand275
fine aggregate. This amount of NBC (0.25% of total aggregate)
therefore would not cause expansion of the AC mixture; most NBC particles would be is very low and therefore
would by
coated notthe
cause expansion
binder materialof(bitumen)
the AC mixture; most NBC
and eliminate their particles
swelling would
capacity. beItcoated
is worth by
the binder material (bitumen) and eliminate their swelling capacity.
mentioning that the AC weight loss percentage is in line with the findings of Naik et al. It is worth mention-
ing that
(2003) forthe AC weight
modified pavinglossstone
percentage
subjected is in
toline with the
FT cycles, findings
which of Naik
revealed et al.
a 0.2% (2003)loss
weight for
modified
for paving
all mixtures stone subjected to FT cycles, which revealed a 0.2% weight loss for all
[38–40].
mixtures [38–40].
Moreover, in terms of stability for specimens modified with NBC and without FT
effect,Moreover,
all specimensin terms
passedof stability
the minimum for specimens modified
requirement; with NBC
however, afterand without
8 weeks FT
of FT
effect, all specimens passed the minimum requirement;
cycles, control specimens and modified specimens with 20% NBC failed the minimumhowever, after 8 weeks of FT cy-
cles, control specimens
requirement, and modified
whereas modified specimensspecimens with10%,
with 5%, 20% andNBC15failed
% of the
NBC minimum
passed the re-
quirement,requirement
minimum whereas modified with 6.1,specimens
7, and 5.3 with
kN,5%, 10%, and 15Therefore,
respectively. % of NBCconsideration
passed the min- of
imum
5% NBC requirement
replacement with
of the6.1,mineral
7, and 5.3 kN,
filler of respectively. Therefore,
aggregate gradation willconsideration
result in minimum of 5%
NBC replacement
weight loss, minimum of thedamage,
mineraland fillermore
of aggregate gradation
stability than requiredwillafter
result8 weeks
in minimum of FT
weight loss, minimum damage, and more stability than required
cycle effect. This is credited to the NBC having a larger surface area than the limestone after 8 weeks of FT cycle
filler and aggregate, meaning that the latter had less contact area with bitumen:filler
effect. This is credited to the NBC having a larger surface area than the limestone the
and aggregate,
cause meaningatthat
of lower reaction the the latter between
interface had less limestone
contact area with bitumen:and
filler–aggregate the bitumen
cause of
lowerthat
than reaction
of NBC at the
andinterface
bitumen.betweenSince NBC limestone filler–aggregate
has a net negative charge,and bitumen than that
polar fractions in
of NBC and
bitumen werebitumen.
adsorbed Since
to theNBC NBC hassurface
a net negative
and formed charge, polarlayer,
a double fractions
whichin resulted
bitumen
were adsorbed to the NBC surface and formed a double layer, which resulted in lower
Coatings 2022, 12, 1664 11 of 14

in lower tensile strength at the interface between binder and aggregate and a decrease in
interlocking of coarse aggregate. Therefore, friction and mechanical interlock will decay
between coarse and fine aggregate in AC when NBC content is increased above 15%. This
finding helped conclude that increasing NBC content in asphalt mixtures causes a reduction
in adhesion between film thickness and coarse aggregate. Notably, size gradation and
morphology of the aggregate and its location in the AC have an impact on aggregate
movement displacement, aggregate skeleton stability, cracking distribution, and fracture
damage of asphalt mixtures at low temperatures [40–42].
In order to establish a relationship between influence of NBC content on average veloc-
ity and the damage index, a comprehensive analysis was conducted. Linear relationships
were established between average velocity and the damage index versus number of weeks
for specimens that were subjected to FT cycles at different NBC contents. The coefficient
of determination (R2 ) was used to access quality of linear fit. R2 is known as a numerical
value that implies the amount of variance explained by the independent variable(s) in the
model. This coefficient of determination was calculated by the following equation:
2
SST − SSR ∑ (Yi − Yp)
R2 = = 1− 2
(2)
SST ∑ (Yi − Yavg)

where R2 = regression model fitting parameter, SSR = sum of squares of errors (residuals),
SST = total sum of squares around the mean, Yi = actual dependent variable acquired
from experimental work, Yp = predicted dependent variable obtained from the regression
model, and Yavg = average value of the actual dependent variable acquired from the
experimental study. Developed linear models between average velocity, number of FT
weeks, and the damage index versus number of FT weeks at different NBC contents, along
with their respective R2 values, are tabulated in Tables 4 and 5, respectively. Based on
the developed models, it can be seen that the established linear models clearly explain
variation in dependent variables (average velocity and damage index) at 95% or better. In
addition, it was observed analytically that NBC content played a significant role in AC
mixture performance under different FT cycles.

Table 4. Developed linear models between average velocity and number of FT weeks.

NBC Content R2
Linear Model (y = Average Velocity, x = Number of FT Weeks)
(%) (%)
0 y = −0.1011x + 3.2028 95.87
5 y = −0.1006x + 3.4438 99.60
10 y = −0.1268x + 3.1535 97.40
15 y = −0.1082x + 3.0239 98.94
20 y = −0.1038x + 3.362 97.33

Table 5. Developed linear models between damage index and number of FT weeks.

NBC Content R2
Linear Model (y = Damage Index, x = Number of FT Weeks)
(%) (%)
0 y = 0.0527x + 0.0403 95.65
5 y = 0.0498x + 0.0364 99.63
10 y = 0.0588x + 0.1166 96.76
15 y = 0.063x + 0.0072 98.87
20 y = 0.0555x + 0.0045 96.42
Coatings 2022, 12, 1664 12 of 14

In general, the performance of asphalt mixtures determines road-pavement perfor-

mance, especially when pavement is exposed to water through its porous medium; water
in porous materials not only causes physical degradation but also carries aggressive agents
such as carbon dioxide (CO2 ), chloride, and sulfates, which can lead to chemical degra-
dation and severely reduce the durability of AC mixtures [43,44]. In addition to that, the
FT effect on AC is a significant parameter that contributes to road-pavement damage.
Marshall-test and UPV measurements were used to evaluate the impact of FT cycles on AC
mixture performance. The two methods were relatively independent and the relationship
between the characterization indexes of the two tests was considered to establish more
comprehensive consideration of bentonite’s improvement of AC mixture performance.
To that end, a single-factor analysis of variance (ANOVA) was carried out; NBC content
was used as the factor based on which comparison was conducted versus flow, stability,
average velocity, and damage index at 0 weeks of FT cycles and flow, stability, average
velocity, and damage index after 8 weeks of rapid and continuous FT cycles. Results are
presented in Tables 6 and 7; Table 6 presents descriptive statistics for the variables used in
the ANOVA and Table 7 shows single-factor ANOVA results. It can be statistically seen,
as was graphically proven, that bentonite content significantly affected all test indexes on
the 0.05 significance level, which supports the motivation of this research. It is of great
importance to point out that the p-Value resulted as <0.0001, which implies that NBC has a
high influencing effect on asphalt-mixture behavior under FT cycles. This in turn indicates
that modifying AC with NBC could help mixtures’ weather-resistance under repeated
cycles of FT in addition to wetting and drying.

Table 6. Single-factor ANOVA results.

Groups Count Sum Average Variance

Bentonite
40 400 10 51.28205
Content (%)
Test Indexes 40 151.8697 3.796742 9.352331

Table 7. Single-factor ANOVA results.

Source of Variation SS df MS F p-Value F Crit

Between Groups 769.61 1 769.61 25.39 2.96 × 10−6 3.96
Within Groups 2364.74 78 30.32
Total 3134.35 79

5. Conclusions
Asphalt concrete mixtures made of asphalt (binder) and aggregate are frequently
applied in construction of flexible pavements to be used in parking lots, airports, roads,
and highways. These pavements are subjected to damage when exposed to FT conditions
over different periods of time (FT cycles), which costs governments and private sectors
billions of dollars and may result in loss of lives every year in several countries around
the world. This research was focused on minimizing this type of damage by using natural
bentonite clay in asphalt concrete modification. Based on the experimental results in this
study, the following conclusions can be made:
(1) FT cycles reduce weight, stability, and velocity in asphalt concrete mixtures.
(2) Adding 5% of NBC in asphalt concrete mixtures in the form of partial replacement
of mineral filler in the aggregate satisfies asphalt-mixture requirements for medium
traffic conditions.
(3) Adding 5% of NBC in asphalt concrete mixtures in the form of partial replacement of
mineral filler in the aggregate reduces damage caused by 8 continuous weeks of rapid
freezing and thawing cycles by 13% as compared to control/unmodified specimens.
Coatings 2022, 12, 1664 13 of 14

Additionally, it provides the smallest amount of AC pavement weight loss (0.25%)

after 8 continuous weeks of rapid FT cycles (one FT cycle is 4 h).
(4) Modifying AC mixtures by available and inexpensive NBC will lead to reduced
maintenance cost.
(5) In the future, improved AC mixtures can be applied in cold regions that suffer the con-
sequences of FT cycles on pavements. They can contribute to reduction of pavement
damage, thus prolonging its service life.

Author Contributions: Methodology, M.I.B.B. and R.M.A.; validation, M.A.K.; formal analysis,
M.I.B.B.; investigation, M.I.B.B.; data curation, R.M.A.; writing—original draft preparation, M.I.B.B.;
writing—review and editing, M.I.B.B.; visualization, M.A.K.; project administration, R.M.A. All
authors have read and agreed to the published version of the manuscript.
Funding: The authors would like to acknowledge the support of Al-Zaytoonah University of Jordan
for research grant number 17/18/2018-2019.
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: Not applicable.
Conflicts of Interest: The authors declare no conflict of interest.

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