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The CA measurement by SD method showed high variability compared to the WP method.
The SFE of asphalt measured by the SD method had higher values than that of WP.
SD method found to be less sensitive to capture acidic component of SFE of asphalt.
CR value of 0.25 by SD method would be approximately equal to 0.5 by WP method.
a r t i c l e
i n f o
Article history:
Received 2 November 2015
Received in revised form 26 February 2016
Accepted 14 March 2016
Keywords:
Surface free energy
Moisture damage
Compatibility
Moisture susceptibility
Wilhelmy plate
Sessile drop
a b s t r a c t
The present study compares two techniques namely Wilhelmy plate (WP) and Sessile drop (SD) methods
to rank moisture damage susceptibility of twelve different asphalt-aggregate combinations. Three asphalt
binders: unmodified (VG30), polymer modified (PMB40), and crumb rubber modified (CRMB60) binders,
and four aggregates (basalt, limestone, granite, and sandstone) were selected in this study. The contact
angle of selected asphalt binders was measured using both WP and SD techniques. Thereafter, surface
free energy (SFE) components of asphalt binders, bonding energy and compatibility ratio (CR) of selected
asphalt-aggregate combinations were estimated. The results showed that the SD method showed a high
variability in measurement of contact angle of asphalt binders compared to the WP method. The SD
method found to be less sensitive to capture acid component of SFE of asphalt binders. Both the methods
showed that PMB40-basalt, VG30-basalt, PMB40-limestone combination can have least susceptible to
moisture damage. However, in majority of the cases (9 out of 12 asphalt-aggregates combinations,
excluding PMB40-basalt, VG30-basalt, PMB40-limestone), both the methods resulted in different moisture damage ranking of asphalt-aggregates combinations. Currently set a minimum threshold value of
CR as 0.5 based on the WP method for screening moisture damage susceptibility of asphalt-aggregate
combination may not be applicable to the SD method. The present study develops a correlation between
the CR of asphalt-aggregate combination estimated from the WP and SD methods.
2016 Elsevier Ltd. All rights reserved.
1. Introduction
The moisture damage causes premature failure of asphaltic
pavements. Many laboratory test methods namely, retained indirect tensile strength ratio, Hamburg wheel tracking, water immersion have been developed to evaluate moisture susceptibility of
asphalt mixes. Though these tests are simple and easy to conduct,
they exhibited a poor correlation with field performance [1,2]. Further, none of these tests describe a mechanism behind bonding and
debonding of aggregates-asphalt system [1,2]. Recently, research Corresponding author.
E-mail addresses: ayyanna.habal@gmail.com (A. Habal), dvsingh@civil.iitb.ac.in
(D. Singh).
http://dx.doi.org/10.1016/j.conbuildmat.2016.03.060
0950-0618/ 2016 Elsevier Ltd. All rights reserved.
ers reported that surface free energy (SFE) of asphalt binder and
aggregates can be a promising parameter in identifying a moisture
resistant mix [38]. The SFE of aggregate and asphalt binder is used
to estimate dry and wet adhesion energy and compatibility ratio
(CR) to evaluate moisture susceptibility of asphalt mixes. The SFE
of asphalt binder is estimated based on measurement of contact
angle. The two methods namely, Wilhelmy plate (WP) and Sessile
drop (SD) are being successfully used by many researchers to measure contact angle of asphalt binders [1,4,6,9,10]. Both the WP and
SD methods have different principle of measuring contact angle of
asphalt binders. For example, WP method measured dynamic contact angle derived by principle of force difference, whereas the SD
method measures static contact angle based on an image of a drop.
352
c cLW cAB
p
where; cAB 2 c c
W BB 2cB
q
q
q
LW
W AB 2 cLW
cA cB 2 cA cB
A cB 2
where, cLW
and cLW
A
B = Lifshitz-van der Waals component of aggre
gate and asphalt binder, respectively, c
A and cB Lewis acid compo
nent of aggregate and asphalt binder, respectively, and, c
A and cB
Lewis base component of aggregate and asphalt binder,
respectively.
2.1.3. Wet adhesion energy wwet
ABW
The presence of water makes coating of asphalt binder to sepa
rate from aggregate. The wet adhesion energy W wet
ABW of asphaltaggregate combination can be estimated using Eq. (5) [1].
W wet
ABW cAW cBW cAB
where, cAW , cBW , and cAB are interfacial energy between aggregatewater, asphalt binder-water and aggregate-asphalt binder,
respectively.
1.1. Objectives
The objectives of this research were to:
Compare contact angle and SFE components of polymer modified, crumb rubber modified and unmodified asphalt binders
measured using the WP and SD methods.
Compare bonding compatibility of modified and unmodified
asphalt binders with four different aggregates (basalt, limestone, granite and sandstone) using dry adhesion energy, wet
adhesion energy and CR estimated from the WP and SD
methods.
Determine moisture susceptibility rank of different combinations of asphalt binders and aggregate based on CR value estimated from the WP and SD methods.
W W
AB
BB
CR
W wet
ABW
353
shown in the experimental plan (Fig. 1), the first step was to measure contact angles
of the selected asphalt binders using the WP and SD methods, and estimating the
SFE components. The SFE components of selected aggregates were adopted from
the literature [4]. Thereafter the following parameters: dry adhesion energy, wet
adhesion energy and CR were estimated for each combination of selected asphalt
and aggregate.
3.1. SFE of asphalt binders
The SFE of asphalt binder can be estimated based on its contact angle. The contact angle of asphalt binders were measured using the WP and SD methods. The
contact angles of binders should be measured using at least three probe liquids of
known SFE components. In this study, three probe liquids namely: distilled water,
glycerol and formamide were used [3,7,11,12,15] to measure contact angle of
selected asphalt binders. Thereafter, the SFE components of asphalt binders were
calculated using the acid-base theory (Eq. (8)). Many of the recent studies reported
SFE measurement of unaged asphalt samples [1,3,57,911,15], considering that
initial coating/bonding of asphalt binder over aggregates occurs at the initial stage
of mix production, prior to start of aging of binder. Thus, SFE of unaged asphalt binders was measured in the present study.
3.1.1. Wilhelmy plate (WP) method
The WP method measures dynamic contact angle of asphalt binders. The DCAT11 instrument from Dataphysics was selected in this study. The device was calibrated with standard probe liquids to ensure its proper working conditions. The
Fig. 2a shows schematic of the WP device. The microscope cover glass plates of size
24 mm 50 mm 0.15 mm were coated with asphalt binder. The asphalt coated
glass plate was immersed into a selected probe liquid (i.e. distilled water, glycerol,
and formamide) at constant speed of 40 lm/s at room temperature. Change in force
(DF) was measured, which is used to estimate dynamic contact angle (h) between
asphalt coated glass plate surface and a probe liquid using Eq. (7) [1]. A minimum
of four replicate of asphalt binder samples with each probe liquid were tested for
contact angle. Thereafter, the SFE components of asphalt binders were estimated
using the acid-base theory (Eq. (8)) [14].
cos h
DF V im ql qair g
Pt cTot
L
0:5cli 1 cos hi
cLW
cLW
s
li
cli cs
p
cli cs
Fig. 2. (a) Schematic diagram of the WP device, and (b) the SD device and contact angle measurement from a typical image.
354
Table 1
The SFE components of aggregates from literature [4].
Basalt
Limestone
Granite
Sandstone
cLW (non-polar)
c+ (acid)
c (base)
cAB (polar)
cTotal
52.3
44.1
48.8
58.3
0.64
2.37
0.00
14.60
164
259
412
855.0
20.49
49.55
0.00
223.5
72.8
93.6
48.84
281.8
Contact angle ()
Aggregate
type
102.297.2
105.9
96.8
104.498.5
80
60
WP
40
SD
20
where, hi = Contact angle of ith probe liquid. Superscript LW, + and indicates
Lifshitz-van der Waals, Lewis acid and Lewis base components, respectively. Subscript li indicates ith probe liquid and subscript s refers to the solid surface.
100
VG30
PMB40
CRMB60
Contact angle ()
(b) Formamide
89.7
84.1
89.6 89.9
93.4
87.7
80
60
WP
40
SD
20
0
VG30
PMB40
CRMB60
(c) Glycerol
120
Contact angle ()
100
89.5 92.6
90.7 93.8
95.5 96.3
80
60
WP
40
SD
20
0
VG30
PMB40
CRMB60
Fig. 3. Contact angle of asphalt binders measured for (a) distilled water, (b)
formamide, and (c) glycerol.
355
(a) LW component
(a) Basalt
24.14
23.46
20
WP
SD
10.72
10
4.87
3.35
PMB40
CRMB60
4.87
4.17
WP
SD
2.68
2.38
2
0.97
VG30
PMB40
70.7
76.4
60
WP
40
SD
20
0
CRMB60
100
VG30
PMB40
107.9
CRMB60
103.6
80.6
75.6
80
85.7 88.6
60
WP
40
SD
20
0
VG30
PMB40
CRMB60
(c) Granite
4.90
WP
SD
2.20
2
0.56
0.29
PMB40
CRMB60
0.08
0
VG30
140
120
100
80
60
40
20
0
125.0
200
183.0
20
14.59
10.90
10
9.23
11.00
94.8
WP
SD
0
PMB40
76.2
89.7
WP
SD
VG30
PMB40
CRMB60
(d) Sandstone
5
VG30
120.7
80.1
25.85
25.29
25
CRMB60
Fig. 4. The SFE components of asphalt binders (a) LW (b) basic (c) acidic, and (d)
total SFE.
87.5
80
120
6.00
15
90.2
81.6
30
91.7
(b) Limestone
6.63
100
VG30
6.14
30
Basic component,mJ/m2
LW component, mJ/m2
170.6
137.1
150
107.2
113.6
122.6
WP
100
SD
50
0
VG30
PMB40
CRMB60
Fig. 5. Dry adhesion energy of asphalt binders with: (a) basalt, (b) limestone, (c)
granite, and (d) sandstone.
-50
-52.8
-47.1
-44.9
-37.5
-40
-30
-25.1
WP
-22.1
-20
SD
-10
VG30
PMB40
CRMB60
(b) Limestone
-100
(a) Basalt
-60
-83.2
-83.1
-78.9
-80
-63.5
-60
-44.0
-43.8
WP
-40
SD
-20
0
VG30
PMB40
CRMB60
(c) Granite
-120
-113.9
-112.5
-100
-107.9
-84.4
-80
-60
-57.0
-56.9
WP
-40
SD
-20
0
VG30
356
-80
PMB40
CRMB60
(d) Sandstone
-70.8
-76.1
-67.3
-60.0
-60
-44.4
-42.6
-40
WP
SD
-20
0
VG30
PMB40
CRMB60
Fig. 6. Wet adhesion energy of asphalt binders with: (a) basalt, (b) limestone, (c)
granite and (d) sandstone.
Aggregate
CR ratio
Individual
ranking
Overall
ranking
WP
VG30
Basalt
Limestone
Granite
Sandstone
2.79
1.96
1.81
1.20
SD
WP
SD
WP
0.66
0.36
0.26
0.26
1
2
3
4
1
2
3
3
2
3
4
6
2
6
7
7
PMB40
Basalt
Limestone
Granite
Sandstone
3.24
1.94
1.80
1.07
0.79
0.56
0.42
0.40
1
2
3
4
1
2
3
3
1
3
4
7
1
3
5
5
CRMB60
Basalt
Limestone
Granite
Sandstone
1.45
1.00
0.86
0.65
0.80
0.47
0.35
0.34
1
2
3
4
1
2
3
3
5
8
9
10
1
4
6
6
SD
0.9
CR (SD method)
Excluded
0.6
0.3
y = 0.1571x + 0.1805
R = 0.586
0
0.5
1.5
2.5
3.5
CR (WP method)
Fig. 7. Correlation between CR values estimated from WP and SD methods.
357
5. Conclusions
Table 2 presents the ranking of different asphalt binderaggregate combinations based on CR estimated from the WP
358
The SD method showed high variability in measurement of contact angle of asphalt binder compared to the WP method. This
variability may be due to difference in method of measurement,
preparation of sample, and principle to estimate contact angle.
The SD method showed higher value of SFE components for an
asphalt binder than that of the WP method except for acidic
components. The SD method found to be less sensitive to capture acidic component of asphalt binders.
The WP method estimated higher dry adhesion energy for a
selected asphalt-aggregate combination compared to the SD
method. Both the WP and SD methods showed different trend
of dry adhesion energy. The WP method ranked VG30 to have
the highest dry adhesion energy, while the SD method ranked
CRMB60 to have maximum dry adhesion energy.
The SD method estimated high wet adhesion energy for a
selected asphalt-aggregate combination compared to the WP
method. Both the methods showed different trend in wet adhesion energy. The WP method showed CRMB60 to have the highest wet adhesion energy, while the SD method showed PMB40
to have the maximum wet adhesion energy.
The CR value for a selected asphalt-aggregate combination calculated based on the WP method was higher than the SD
method. Based on CR value, it was noticed that both the WP
and SD methods showed opposite trend for limestone, granite,
and sandstone aggregates.
The CR value of 0.25 estimated from the SD method would be
approximately equal to a CR of 0.5 estimated from the WP
method.
The WP and SD methods showed that basalt aggregate may give
a better bond with selected asphalt binders in this study, while
sandstone aggregates may result in a poor bond for selected
binders.
The PMB40-basalt, VG30-basalt, PMB40-limestone combination
were ranked 1, 2, and 3, respectively by both the WP and SD
methods. However, it was found that in majority of asphaltaggregate combinations selected in the present study, both
the WP and SD methods provided different ranking.
The outcome of the present study may not be generalized,
because the other factors such as aging and chemical composition
of binders play important role in SFE characteristics. It is recommended that a future study be conducted to evaluate and validate