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To cite this article: Francesco Canestrari , Fabrizio Cardone , Andrea Graziani , Felice Ausilio Santagata & Hussain
U. Bahia (2010) Adhesive and Cohesive Properties of Asphalt-Aggregate Systems Subjected to Moisture Damage, Road
Materials and Pavement Design, 11:sup1, 11-32, DOI: 10.1080/14680629.2010.9690325
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Adhesive and Cohesive Properties
of Asphalt-Aggregate Systems Subjected
to Moisture Damage
Hussain U. Bahia**
ABSTRACT. The bond strength between asphalt and aggregate plays a fundamental role in
evaluating the moisture sensitivity of HMA Mixtures. In this study the effect of water on
adhesive and cohesive properties of asphalt-aggregate systems was investigated using a
modified version of the PATTI. The device was used to measure the pull-off strength on
different asphalt-aggregate combinations and to evaluate the influence of water immersion at
two different temperatures. In particular, six asphalt binders were employed in combination
with two aggregate types, having different asphalt affinity. The effect of the aggregate surface
temperature during specimen preparation was also tested. In the first phase of the study the
within-laboratory repeatability of the test procedure was investigated. The results showed the
PATTI test is able to evaluate with good precision the pull-off strength and that its
repeatability depends on the failure type (adhesive or cohesive). In the second phase of the
study a full factorial experiment was employed to verify the reliability of the test for routine
use in determining the adhesive and cohesive properties of asphalt-aggregate combinations
and the effects of moisture damage. The results showed that, in the dry condition, the test was
able to measure the internal cohesion of the asphalt binders. The results also showed the
effects of water damage on the pull-off strength and the decisive role of asphalt-aggregate
affinity was clearly highlighted. Using wet conditioning of the PATTI samples it was proven
that water affects the adhesive bond between asphalt and aggregate much more than the
asphalt cohesion. Moreover, the results indicate that aggregate temperature during sample
preparation has only a limited effect on the adhesive strength.
KEYWORDS: Asphalt Binder-aggregate Interaction, Moisture Sensitivity, Pull-off Test,
Adhesion, Cohesion.
DOI:10.3166/RMPD.11HS.11-32 2010 Lavoisier, Paris
1. Introduction
Research objectives
The experimental study presented in this paper was focused on the evaluation of
the PATTI device as a routine test for determining the adhesive and cohesive
properties of asphalt-aggregate combinations and the effects of moisture damage on
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them. The pull-off strength and its reduction, produced by the immersion in water,
were used to assess the effects of moisture damage, with reference to the failure
mechanism (adhesive or cohesive).
The experimental investigation was organized in two phases and a statistical
analysis was performed in order to obtain a first estimation of the test repeatability
and to evaluate the significance of each test factor on the pull-off strength.
PULLING FORCE
REACTION PLATE
GASKET GASKET
PISTON
PRESSURE
HOSE
xxxx
xxxx
xxxx
xxxx
xxxx
xxxx
xxxx
xxxx
xxxx
xxxx
xxxx
PULL-STUB
AGGREGATE SURFACE
COATING
preparation, the hot asphalt flow out as the pull-stub was pressed on the aggregate
surface. This resulted in a decrease of the adhesion area between the asphalt and the
steel surface of the pull-stub. As a consequence the failure often occurred at the
asphalt-steel interface and was not representative of the real adhesion and/or
cohesion strength of the asphalt-aggregate system.
In this study a modified version of the PATTI set up was used (Santagata et al.,
2009). The head of the pull-stub was improved with a 200 m thick perimetrical
edge. This provided the necessary lateral confinement for the asphalt binder during
the specimen preparation. Moreover, eight cuts made along the edge allowed the
excess asphalt binder to flow out as the stub was pressed on the aggregate surface.
An excellent control of the asphalt film thickness was obtained so guaranteeing a
complete adhesion between the asphalt and metal pull-stub. Figure 2 shows the
details of the modified pull-stub and the specimen set up.
With these improvements the PATTI results became more reliable and the device
a practical tool to evaluate the adhesion/cohesion properties of asphalt-aggregate
system and the effects of moisture damage (Santagata et al., 2009).
Perimetrical cuts
External edge
200 Pm thick
3. Experimental program
3.1. Materials
Two plain asphalt binders and four polymer-modified binders were used in this
study. The plain binders had different penetration grade, 50/70 pen and 70/100 pen
respectively. The modified binders were obtained by modifying base binders, CRM
and FH, containing two different asphaltene contents: 9% and 16.25% respectively.
Each binder was modified with 0.7% Elvaloy polymer and with 2% SBS Linear
polymer.
Two aggregate types with different binder affinity were selected as substrate.
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The first was a fairly compact limestone which was known to have good asphalt
affinity and the second was a porphyry aggregate
The asphalt binder was heated to 135 C to reach the required viscosity and
perfectly adhere to the metal pull-stub which was immediately pressed onto the
aggregate surface (Kanitpong et al., 2003; Santagata et al., 2009).
The aggregate specimens were prepared by saw cutting in small plates,
approximately 5 mm thick. Before pressing the pull-stub, the surface of the
aggregate plates were cleaned and dried by heating for 12 hours using an oven. Prior
to testing the specimens were conditioned for 24 hours in different environments.
All the pull-off tests were performed at 25 C.
The precision of the test procedure was initially investigated through the
evaluation of the within-laboratory repeatability (ISO 1994). Four samples were
prepared, employing two modified asphalt binders, CRM Elvaloy and FH SBS,
in combination with the two selected aggregate types (limestone and porphyry).
Moreover, the aggregate surface was heated at two different temperatures, 90 C and
135 C. Fifteen replicates were prepared for each test sample, resulting in a total of
60 specimens. The pull-off tests were carried out after conditioning by immersion in
distilled water at 25 C.
In the second phase, the reliability of the test procedure for routine use was
investigated. A full factorial experiment was designed to include twelve asphalt-
aggregate combinations (six binders and two aggregates), two aggregate surface
temperatures (90 C and 135 C) and three conditioning environments:
1) in air, at 25 C (dry condition);
16 Road Materials and Pavement Design. EATA 2010
4. Analysis of results
The failure mechanism was visually investigated after each test and recorded as
one of three major failure types. If the aggregate surface remained completely
coated by the binder (Figure 3a) it was assumed that failure occurred inside the
asphalt film and was thus denoted as purely cohesive (C). In this case asphalt-
aggregate adhesion strength exceeded the binder pulling strength or internal
cohesion. If the aggregate surface remained clean after the test (Figure 3b) it was
assumed that failure occurred at the asphalt-aggregate interface and was denoted as
adhesive (A). When the aggregate surface remained partially coated with asphalt,
the failure could not be defined as (purely) cohesive or (purely) adhesive. A third
type was therefore identified as cohesive-adhesive for this hybrid failure type (C/A),
(Figure 3c).
Pull-off strength
Binder type Test variables Failure type Average Std.Dev. CoV
C A C/A kPa kPa %
1
S2 xi2 ( xi )2 [1]
n
n n
k
[2]
b an i 1(xn i 1 xi )
i 1
18 Road Materials and Pavement Design. EATA 2010
where k=n/2 if n is even, or k=(n-1)/2 if n is odd, and the an-i+1 are tabled in function
of n (Shapiro, 1997).
Then, the test statistic W was calculated:
2
b
W [3]
calc 2
S
Finally, the Wcalc value was compared with a theoretical Wtab determined as a
function of the sample size (n) and for a 5% significance level. When the calculated
value Wcalc is greater than Wtab the hypothesis of normality is accepted.
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The results of the Shapiro-Wilk test are summarized in Table 2. The Wcalc is
greater than the tabled Wtab for 3 of the 4 test conditions. Only the sample obtained
with the FH-SBS asphalt in combination with porphyry at 90 C, did not comply
with the normal distribution. In this case, where only purely adhesive failure were
observed, the distribution was in fact negatively skewed, presenting a longer tail on
the left side (lower values of the pull-off strength).
2 2
H : V V [4]
0 x y
If the sample variances S2x and S2y are considered, then test statistic F can be
calculated as follows:
S2
x
F [5]
S2
y
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Following the Fischer distribution, with n-1 and m-1 degrees of freedom, the
Null Hypothesis H0 is rejected if:
S2 S2
x x
! F or if F [6], [7]
2
S D / 2, n 1, m 1 S2 1 D / 2, n 1, m 1
y y
where FD/2, n-1, m-1 and F1-D/2, n-1, m-1 are the upper and lower 100D/2 percentage points
of the Fischer distribution, and Dis the significance level (5%). The F-test results
are summarized in Table 3.
Binder type Test conditions Hypothesis Test Binder type Test conditions Hypothesis Test
failures the Null Hypothesis is accepted. This means that these variances cannot be
considered statistically different and a combined repeatability standard deviation can
be computed for purely cohesive or hybrid failures:
r 1.96V 2 [9]
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where 1.96 is the value of the standard normal distribution (Z) corresponding to a
95% probability level, and V is the population standard deviation. SinceV is
unknown, the sample standard deviation sr estimated above is used. Hence, for
purely cohesive or hybrid failures we obtain:
cohesive strength. This could be identified as the upper limit of the adhesive strength
as far as porphyry aggregate are considered.
Asphalt 70/100
Aggregate
No immersion Conditioning @25C Conditioning @40C
Type and
Temperature Average Std.Dev. Average Std.Dev. Average Std.Dev.
Failure Failure Failure
(kPa) (kPa) (kPa) (kPa) (kPa) (kPa)
Limestone
2693 328 C 2628 153 C 1708 459 C/A
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T=135C
Limestone
3010 141 C 2076 152 C/A 1864 156 C/A
T=90C
Porphyry
2746 194 C 1340 63 C/A 1019 247 A
T=135C
Porphyry
2695 164 C 889 188 A 747 131 A
T=90C
Asphalt 50/70
Aggregate
Type and No immersion Conditioning @25C Conditioning @40C
Temperature Average Std.Dev. Average Std.Dev. Average Std.Dev.
Failure Failure Failure
(kPa) (kPa) (kPa) (kPa) (kPa) (kPa)
Limestone
3160 486 C 2342 224 C/A 1004 169 C/A
T=135C
Limestone
3654 154 C 2121 97 C/A 1108 153 C/A
T=90C
Porphyry
3172 528 C 1994 396 C/A 658 103 C/A
T=135C
Porphyry
3456 114 C 950 70 A 716 54 C/A
T=90C
Limestone
1856 126 C 1599 198 C 862 168 C/A
T=135C
Limestone
1813 116 C 1767 106 C 1496 211 C
T=90C
Porphyry
1957 198 C 1185 224 C 915 201 C/A
T=135C
Porphyry
1837 181 C 752 23 A 798 87 A
T=90C
22 Road Materials and Pavement Design. EATA 2010
Table 4 (Continued). Pull-off strength results for the investigated asphalt binders
Limestone
2176 96 C 2288 156 C 1518 256 C/A
T=135C
Limestone
2359 115 C 2089 253 C 1471 182 C/A
T=90C
Porphyry
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Porphyry
2009 148 C 576 94 A 476 107 A
T=90C
Limestone
2936 128 C 3244 266 C 2253 126 C
T=135C
Limestone
2745 108 C 2491 154 C/A 1941 36 C
T=90C
Porphyry
3160 184 C 1213 249 C/A 1373 220 C
T=135C
Porphyry
2905 213 C 816 63 A 882 69 A
T=90C
Limestone
3460 106 C 2987 44 C 2443 206 C/A
T=135C
Limestone
3399 112 C 2695 214 C/A 2508 124 C/A
T=90C
Porphyry
3332 96 C 982 92 A 679 174 A
T=135C
Porphyry
3678 118 C 569 117 A 542 51 A
T=90C
The data precision, in terms of repeatability, was comparable with the values
estimated in phase I. Only 5 out of 56 samples characterized by a cohesive or hybrid
failure showed a standard deviation that was significantly higher than 200 kPa. The
pull-off values characterized by adhesive failures had a generally higher variability.
Moisture Damage of Asphalt-Aggregate System 23
800
Adhesive Failure - Porphyry Cohesive Failure - Limestone
500
400
300
200
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100
0
0 500 1000 1500 2000 2500 3000 3500 4000
Figure 4. Pull-off strength results for all binder illustrating the failure type
In Figure 5 the test results were divided for each asphalt with highlighting the
other test variables. This graphical representation is more suitable for a clear
analysis of the data and for highlighting the effects of moisture damage.
3000
Pull-off strength (kPa)
2000
Hybrid or
cohesive failure
1000
Adhesive failure
0
No conditioning Conditioning Conditioning No conditioning Conditioning Conditioning
@25C @40C @25C @40C
Conditioning
Porphyry 135C Porphyry 90C Limestone 135C Limestone 90C
Figure 5a. Pull-off strength results for each binder illustrating the moisture
conditioning effects
24 Road Materials and Pavement Design. EATA 2010
4000
Asphalt CRM Elvaloy Asphalt CRM-SBS
3000
Pull-off strength (kPa)
2000
Hybrid or
cohesive failure
1000
Adhesive failure
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0
No conditioning Conditioning Conditioning No conditioning Conditioning Conditioning
@25C @40C @25C @40C
Conditioning
Porphyry 135C Porphyry 90C Limestone 135C Limestone 90C
3000
Pull-off strength (kPa)
2000
Hybrid or
cohesive failure
1000
Adhesive failure
0
No conditioning Conditioning Conditioning No conditioning Conditioning Conditioning
@25C @40C @25C @40C
Conditioning
Porphyry 135C Porphyry 90C Limestone 135C Limestone 90C
Figure 5b. Pull-off strength results for each binder illustrating the moisture
conditioning effects
affected by small departures from normality (Ryan, 2007). Moreover, the results of
Phase I support the assumption of a normal distribution.
The first step in the analysis was to test the assumption of equality of variances,
and this has been performed using Bartletts test. This gave a positive result for all
the asphalt binders. The results of ANOVA are summarized in Table 5. For each
binder and for the two experimental factors (aggregate type and surface
temperature), the test outcome is shown along with the relevant p-value. In nine out
of twelve cases the p-value considerably exceed the significance level D=0.05i.e.
p > D=0.05). This confirmed that in these cases the pull-off strength measured by the
PATTI device after dry conditioning was independent from both the aggregate
surface temperature and aggregate type and therefore could be properly considered a
measure of the binder internal cohesion.
The dry pull-off strength was used to rank the six binders considered in the
study. The average values were reported in Table 6 along with the coefficient of
variation. Table 7 summarizes the results of pairwise comparisons between these
26 Road Materials and Pavement Design. EATA 2010
values performed using the t-test. The results confirmed that the PATTI device was
effective in detecting the effect of both composition and modification agent.
1 2 3 4 5 6
Binder FH-SBS 50/70 FH-Elvaloy 70/100 CRM-SBS CRM-Elvaloy
Table 7. t-test results to evaluate the composition and modification type effect on the
pull-off strength
failures. This could mean that, when a hybrid failure occurs, it begins with an
adhesion loss at a fairly weaker point of the asphalt-aggregate interface. Then, as a
consequence of the reduced bonding area, a greater tensile stress is imposed to the
asphalt film that comes to a cohesive failure.
For specimens conditioned with immersion at 40 C, the t-test revealed that the
surface temperature effect were negligible for both aggregate types (Table 9). In
particular for porphyry samples, where purely adhesive failures were observed, the
effect was so severe that the positive effect of an higher surface temperature was
lost.
28 Road Materials and Pavement Design. EATA 2010
Limestone Aggregate
Water conditioning@25C
Binder type
Significant? p-value Pull-off loss
CRM-Elvaloy YES 0.035 8%
FH-Elvaloy NO 0.820 0%
CRM-SBS NO 0.354 3%
The immersion at 25C of the PATTI specimen had a small effect on the asphalt
internal cohesion. This is clear from analyzing the pull-off strength loss, in
comparison with the dry conditioning, measured on limestone samples (Table 10). A
Moisture Damage of Asphalt-Aggregate System 29
t-test also showed that for two binders (FH-Elvaloy and CRM-SBS) this reduction
was not even significant.
On the other hand immersion at 25 C had a clear effect on adhesion, at least for
the porphyry aggregates. The adhesive strength dropped below the internal cohesion
of the asphalt and a significant reduction of pull-off strength is measured with the
change in failure mechanism: from cohesive to adhesive.
The same phenomena were observed comparing the PATTI results after
immersion at 40 C, with the dry conditioning results (Table 11): water acted mainly
on the asphalt-aggregate adhesive bond. For the porphyry aggregate, this effect was
remarkable and adhesive failures were always observed as the adhesion strength
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dropped below the internal cohesion of the asphalt film. With limestone aggregates,
the loss in pull-off strength was less severe. In fact, because of the better asphalt
affinity, hybrid failures were prevalent.
5. Conclusions
The experimental study presented in this paper was focused on the evaluation of
the modified PATTI device as a routine test for determining the stripping potential
of asphalt-aggregate combinations. Six asphalt binders and two aggregate types
were considered in the study.
The precision of the test procedure was investigated. A statistical analysis
showed that the within-laboratory repeatability is highly dependent on the failure
mechanism.. In the case of cohesive and hybrid failures a repeatability standard
deviation of 200 kPa was estimated.
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The research study also investigated the pull-off strength and its reduction
produced by water immersion in order to assess the effects of moisture damage. All
the tests performed after dry conditioning showed cohesive failures, regardless of
asphalt-aggregate combination or aggregate surface temperature. A statistical
analysis confirmed that, in this case, could the pull-off strength could be considered
a measure of the binder internal cohesion. Tests performed after water immersion
showed that the asphalt-aggregate affinity controls the transition from cohesive to
adhesive failures. With porphyry aggregates adhesive failures were observed for
almost all test conditions, together with a significant drop of strength. With
limestone aggregate purely adhesive failures were never observed, indicating a
better binder affinity.
In general the modified binders used in this study showed a lower water
sensitivity, in terms of cohesion loss. A better asphalt-aggregate affinity was
obtained with the Elvaloy modification compared to the SBS modification.
Moreover, a higher asphaltene content of base binders resulted in a higher cohesive
and adhesive strength.
Considering the overall results of this study, the proposed modified PATTI test is
found to be a repeatable, reliable and practical method to investigate the adhesion
and cohesion properties of asphalt-aggregate bonding. Moreover, its ability to
discriminate between different asphalt-aggregate systems in terms of moisture
sensitivity could prove to be a suitable method for designing asphalt mixtures with
high moisture resistance.
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