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Adhesive and Cohesive Properties of Asphalt-


Aggregate Systems Subjected to Moisture Damage
a a a
Francesco Canestrari , Fabrizio Cardone , Andrea Graziani , Felice Ausilio Santagata
a b
& Hussain U. Bahia
a
Universit Politecnica delle Marche , Via Brecce Bianche, 60100, Ancona, Italy E-mail:
b
University of Wisconsin-Madison , 1415 Engineering Dr, Madison, WI, 53706, USA E-mail:
Published online: 19 Sep 2011.

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

To link to this article: http://dx.doi.org/10.1080/14680629.2010.9690325

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Adhesive and Cohesive Properties
of Asphalt-Aggregate Systems Subjected
to Moisture Damage

Francesco Canestrari* Fabrizio Cardone*


Andrea Graziani* Felice Ausilio Santagata*
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Hussain U. Bahia**

* Universit Politecnica delle Marche


Via Brecce Bianche, 60100 Ancona, Italy
{f.canestrari; f.cardone}@univpm.it
{a.graziani; santafe}@univpm.it
** University of Wisconsin-Madison
1415 Engineering Dr, Madison, WI 53706, USA
bahia@engr.wisc.edu

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

Road Materials and Pavement Design. EATA 2010, pages 11 to 32


12 Road Materials and Pavement Design. EATA 2010

1. Introduction

Moisture damage is a major cause of premature failure in asphalt concrete


pavement as it accelerates or causes some typical pavement distresses such as
bleeding, rutting, cracking, ravelling and potholes (Kiggundu et al. 1988; Terrel et
al. 1994).
Moisture-induced damage consists of a dislodging process of the aggregate from
the HMA pavement under the action of traffic loading (Hicks, 1991, Kandhal, 1994,
Kiggundu et al.,1988, Tunnicliff et al., 1984). This degradation process, commonly
known as stripping, can be regarded as a combination of adhesive and cohesive
failures (Fromm, 1974; Kiggundu et al., 1988; Stuart, 1990, Taylor et al., 1983,
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Terrel et al., 1989).


Adhesive failure is characterized by the separation of the asphalt coating from
the aggregate. It is caused by the action of water at the asphalt-aggregate interface
that weakens the adhesive bond between asphalt and the aggregate surface (Hicks,
1991). Different theories as chemical reaction, molecular orientation, mechanical
adhesion and surface energy are used to explain this adhesion bond (Hefer et al.,
2005).
Cohesive failure is due to the separation of molecules within the asphalt film. In
this case, the water the cohesive bonds within the asphalt binder itself, for example
through an emulsification process. A cohesive failure mechanism can also lead to an
adhesive failure when the emulsification effects reach the aggregate surface
(Fromm, 1974).
The methods for measuring moisture sensitivity of HMA are currently based on
tests performed on asphalt concrete mixtures. Some of these involve visual
inspection (qualitative determinations) of aggregate coating degradation on loose
mixtures after water immersion (e.g. EN 12697-11). Other methods are based on the
comparison of mechanical properties measured on unconditioned and conditioned
compacted samples or through tests that consider the combined interaction of loads,
temperature and moisture (Kim et al., 2006; Lottman, 1982; Solaimanian, 2003;
Stuart, 1990; Terrel et al., 1994; Gubler et al., 2005).
These well recognized methods are likely to measure bulk properties of the
mixture rather than specific changes in the adhesion and cohesion properties of the
asphalt-aggregate system due to the water action. Therefore, it is not surprising that
they cannot be considered sufficient predictors of the cause of HMA stripping.
A better understanding of the moisture sensitivity of HMA could be achieved
with a quantitative measurement of the influence of water on both adhesion and
cohesion, performed directly on the asphalt-aggregate system (Youtcheff, 1997;
Huang et al., 2002; Kanitpong et al., 2003).
This type of measures can be carried out with a simple pull-off test, using a
specific device developed for the coating industry. In particular the Pneumatic
Moisture Damage of Asphalt-Aggregate System 13

Adhesion Tensile Testing Instrument (PATTI), has been proposed by several


Authors to evaluate the adhesive and cohesive properties of asphalt-aggregate
combinations in the presence of water (Youtcheff, 1997; Kanitpong et al., 2003;
Kanitpong et al., 2005; Copeland et al., 2007; Santagata et al., 2009).

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.

2. The testing device

The Pneumatic Adhesion Tensile Testing Instrument (PATTI) was initially


developed by the National Institute for Standardization and Testing (NIST), to
investigate the adhesiveness (or bond) between a paint, coating or general adhesive
and a rigid substrate (Figure 1a).
The PATTI measures the pull-off strength of the coating-substrate system
through the application of a tensile force (ASTM 2002). Its use for the measurement
of the adhesive and cohesive properties of asphalt-aggregate combinations is quite
straightforward.

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

Figure 1. PATTI device (a) and its schematic drawing (b)


14 Road Materials and Pavement Design. EATA 2010

A small asphalt sample is applied on a proper metal pull-stub that is pressed


immediately onto a prepared aggregate surface to establish a good asphalt-aggregate
bond. A self-aligning piston and a reaction plate are screwed to the pull-stub and a
pulling force is exerted using a pneumatic system (Figure 1b). The pulling force is
increased and failure occurs when the adhesive strength of the asphalt-aggregate
system or the cohesive strength of the asphalt is reached. The control module
records the failure force, which is converted into pull-off tensile strength (kPa) as a
function of the bonding surface area.
This test configuration, with minor modifications, was used in several studies
(Youtcheff, 1997; Kanitpong et al., 2003; Kanitpong et al., 2005). It was pointed out
that, at the high aggregate temperature (i.e. 135C and 90C) adopted during sample
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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

Figure 2. Modified pull-stub


Moisture Damage of Asphalt-Aggregate System 15

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

3.2. Specimen preparation and conditioning

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.

3.3. Testing plan

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

2) immersion in distilled water at 25 C for 24 hours;


3) immersion in distilled water at 40 C for 24 hours.
Five replicates were prepared for each of the 72 test combinations, resulting in
testing a total of 360 specimens.

4. Analysis of results

4.1. Failure types


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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).

a) Cohesive b) Adhesive c) Coesive/Adhesive


Figure 3. Type of failures from pull-off tests

4.2. Phase I Testing

4.2.1. Test results


The results of the first phase are summarized in Table 1. The observed failure
type is reported along with the average, standard deviation and coefficient of
variation of the pull-off strength.
For the CRM-Elvaloy binder a cohesive failure was observed in all specimens,
Moisture Damage of Asphalt-Aggregate System 17

while the FH-SBS binder yielded an aggregate-dependent failure. In particular a


purely adhesive failure was observed with the Porphyry aggregate, while with the
Limestone aggregate purely cohesive and hybrid cohesive-adhesive failures were
observed.
In terms of pull-off strength the four samples show a wide range of values, from
544 kPa to 2740 kPa, and had coefficients of variation that range between 8% and
17%.

Table 1. Results of phase I


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Pull-off strength
Binder type Test variables Failure type Average Std.Dev. CoV
C A C/A kPa kPa %

CRM-Elvaloy Limestone - T=135 C 15 0 0 1754 211 12

CRM-Elvaloy Porphyry - T=135 C 15 0 0 1003 170 17

FH-SBS Limestone - T=90 C 5 0 10 2740 216 8

FH-SBS Porphyry - T=90 C 0 15 0 544 80 15

4.2.2. Statistical analysis


A statistical analysis was performed on the data obtained in phase I to get a first
estimation of the precision of the test method. All the tests were performed by the
same operator, with the same apparatus, in similar laboratory conditions and within
the shortest practical period of time, hence a within-laboratory repeatability could
be estimated.
Commonly the normal probability function is used to describe the distribution of
independent random measurements obtained under repeatability conditions. The
hypothesis of normality was verified using the Shapiro-Wilk test (Shapiro, 1997).
For this test, the elements of each sample were initially ordered, from the
smallest to the largest (x1.xn) and the quantities S2 and b were calculated as
follows:

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).

Table 2. Shapiro-Wilk test results

Binder type Test variables S2 b2 W calc W tab


(kPa) (kPa)

CRM-Elvaloy Limestone - T=135 C 621631 609700 0.9808 0.8810

CRM-Elvaloy Porphyry - T=135 C 403328 388960 0.9644 0.8810

FH-SBS Limestone - T=90 C 651732 611846 0.9388 0.8810

FH-SBS Porphyry - T=90 C 90051 76789 0.8527 0.8810

4.2.3. Repeatability standard deviation


The standard deviation values reported in Table 1 can be considered as a first
estimation of the modified PATTI repeatability. The low value obtained for purely
adhesive failures (80 KPa), suggests that a different repeatability should be expected
for this type of failure.
This hypothesis was verified by comparing each couple of sample variances with
an F-test. The test is based on verifying the hypothesis that the variances of two
normal populations Vx and Vy, are equal between them.
Let x1 xn and y1 yn be the random samples of n and m observations from
these populations, respectively. The Null Hypothesis (H0) to be verified is:
Moisture Damage of Asphalt-Aggregate System 19

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.

Table 3. Hypothesis test on variance results

Binder type Test conditions Hypothesis Test Binder type Test conditions Hypothesis Test

CRM-Elvaloy Limestone - T=135 C CRM-Elvaloy Limestone - T=135 C


H 0 accepted H 0 rejected
CRM-Elvaloy Porphyry - T=135 C FH-SBS Porphyry - T=90 C

CRM-Elvaloy Porphyry - T=135 C CRM-Elvaloy Limestone - T=135 C


H 0 rejected H 0 accepted
FH-SBS Porphyry - T=90 C FH-SBS Limestone - T=90 C

CRM-Elvaloy Porphyry - T=135 C FH-SBS Porphyry - T=90 C


H 0 accepted H 0 rejected
FH-SBS Limestone - T=90 C FH-SBS Limestone - T=90 C

Based on the variance estimated for adhesive failures (FH-SBS asphalt in


combination with porphyry at 90C), the Null Hypothesis is always rejected. This
confirms that the repeatability measured for adhesive failures is significantly
different (lower) from the repeatability measured for cohesive or hybrid failures.
Moreover, this result can be considered a strong statistical conclusion for the chosen
D value. (Montgomery et al., 2003).
On the other hand, comparing the repeatability variances for cohesive and hybrid
20 Road Materials and Pavement Design. EATA 2010

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:

sr 200 kPa [8]

This value is considered a first estimation, exclusively when purely cohesive or


hybrid failures are observed. The corresponding repeatability limit can be calculated
as:

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:

r 553 kPa [10]

Similarly, for adhesive failures:

r = 229 kPa [11]

4.3. Phase II testing

4.3.1. Evaluation of the general test results


The results of the second phase, grouped for each asphalt binder, are summarized
in Table 4. The average and standard deviation of five pull-off strength
measurements are reported, along with the predominant failure type. The same test
results were plotted in Figure 4, highlighting the aggregate type.
Some general observations could be made on the pull-off values:
purely adhesive strength varied between 500 kPa and 1100 kPa;
all purely adhesive failures were observed with porphyry aggregates;
purely cohesive strength varied between 1200 kPa and 3700 kPa;
the aggregate type did not seem to influence purely cohesive strength;
all dry conditioned specimen yielded cohesive failures;
for hybrid failures, limestone aggregates generally yielded higher strength than
porphyry aggregates.
The PATTI results confirm the key role of asphalt-aggregate affinity and the
better adhesion provided by limestone aggregates. Moreover, a clear separation, at
approximately 1100 kPa, appeared to exist between purely adhesive and purely
Moisture Damage of Asphalt-Aggregate System 21

cohesive strength. This could be identified as the upper limit of the adhesive strength
as far as porphyry aggregate are considered.

Table 4. Pull-off strength results for the investigated asphalt binders

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

Asphalt CRM 0.7% Elvaloy


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
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

Asphalt CRM 2% SBS Linear


Aggregate Type
No immersion Conditioning @25C Conditioning @40C
and
Temperature Average Std.Dev. Average Std.Dev. Average Std.Dev.
Failure Failure Failure
(kPa) (kPa) (kPa) (kPa) (kPa) (kPa)

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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2425 183 C 1022 125 A 546 60 A


T=135C

Porphyry
2009 148 C 576 94 A 476 107 A
T=90C

Asphalt FH 0.7% Elvaloy


Aggregate Type
No immersion Conditioning @25C Conditioning @40C
and
Temperature Average Std.Dev. Average Std.Dev. Average Std.Dev.
Failure Failure Failure
(kPa) (kPa) (kPa) (kPa) (kPa) (kPa)

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

Asphalt FH 2% SBS Linear


Aggregate Type
No immersion Conditioning @25C Conditioning @40C
and
Temperature Average Std.Dev. Average Std.Dev. Average Std.Dev.
Failure Failure Failure
(kPa) (kPa) (kPa) (kPa) (kPa) (kPa)

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

700 Cohesive Failure - Porphyry Hybrid Failure - Limestone

Hybrid Faiiure - Porphyry Repeatability - Phase I


600
Standard Deviation (kPa)

500

400

300

200
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100

0
0 500 1000 1500 2000 2500 3000 3500 4000

Test Level - Average Pull-Off Strength (kPa)

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.

Asphalt 70/100 Asphalt 50/70


4000

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

Asphalt FH Elvaloy Asphalt FH- SBS


4000

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

4.3.2. Pull-off strength after dry conditioning


In the pull-off tests performed after dry conditioning (24 hours in air @25 C) all
the specimens showed cohesive failures, regardless of asphalt-aggregate
Moisture Damage of Asphalt-Aggregate System 25

combination and aggregate surface temperature. Therefore, without the influence of


water, the asphalt-aggregate adhesive bond is found always higher than the asphalt
film inner cohesion. As a consequence the dry pull-off strength is not found to be
significantly affected by the aggregate surface temperature or the aggregate type.
A one-way ANOVA at 95% confidence level was used to verify this hypothesis.
This procedure is a generalization of the t-test when more than two population
means have to be compared. In this case, for each asphalt binder, the four pull-off
strengths measured after the dry condition were compared. Although each
population should be verified to be normally distributed when ANOVA is used, it is
not practical to test this assumption with only five observations. The assumption that
the data are normally distributed is reasonable since ANOVA is not strongly
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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=0.05 i.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.

Table 5. Results of statistical analysis to evaluate the aggregate surface and


aggregate type on pull-off strength

Aggregate Temperature Aggregate type


Binder type
Significant? p-value Significant? p-value
50/70 YES 0.0444 NO 0.6529
70/100 NO 0.6759 NO 0.0844
CRM-Elvaloy NO 0.2701 NO 0.3929
FH-Elvaloy YES 0.0077 YES 0.0185
CRM-SBS NO 0.7618 NO 0.5136
FH-SBS NO 0.1309 NO 0.6684

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.

Table 6. Binder ranking in terms of dry pull-off strength at 25 C

1 2 3 4 5 6
Binder FH-SBS 50/70 FH-Elvaloy 70/100 CRM-SBS CRM-Elvaloy

Average (kPa) 3498 3360 2936 2716 2329 1866

CoV (%) 5.3 10.8 7.3 8.5 16.6 8.4


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Table 7. t-test results to evaluate the composition and modification type effect on the
pull-off strength

Chemical Composition Modification Type


Pairs of binders Binder type
Significant? p-value Significant? p-value
CRM-Elvaloy CRM-Elvaloy
YES < 0.0001 YES < 0.0001
FH-Elvaloy CRM-SBS
CRM-SBS FH-Elvaloy
YES < 0.0001 YES < 0.0001
FH-SBS F-SBS
50/70 pen
YES < 0.0001
70/100 pen

4.3.3. Effect of water immersion on pull-off strength


The effect of water on the adhesive and cohesive properties of asphalt-aggregate
combinations was evaluated performing PATTI tests after 24 hours of water
immersion at 25 and 40 C.
A decrease of the pull-off strength was generally measured. In many cases a
change in the failure type was also observed as hybrid or purely adhesive failures.
The aggregate type proved to have a major role in this phenomena.
With the porphyry aggregate, an adhesive failure and a significant drop of pull-
off resistance is measured for almost all test conditions, and in particular after
immersion at 40 C. This means that moisture, penetrating through the pores of the
aggregate, and from the sides of the asphalt film, reached the asphalt layer interface
decreasing the adhesion strength to a level below the cohesive strength of the
asphalt.
A purely adhesive failure was not observed with the limestone aggregate,
indicating its better binder affinity. When purely cohesive failures are observed, a
small reduction in pull-off strength is measured, as compared to the corresponding
dry condition, whereas higher reductions in strength are measured for hybrid
Moisture Damage of Asphalt-Aggregate System 27

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.

4.3.4. Effect of aggregate surface temperature


Varying the temperature of the aggregate surface between 90 C and 135 C was
expected to influence the adhesion between asphalt and aggregate, and hence the
moisture susceptibility. Higher surface temperature should result in higher adhesion
values since the lower asphalt viscosity allow better bonding, which should lead to
lower sensitivity to water damage. This hypothesis was tested by performing
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pairwise comparisons with the t-test.


For specimens conditioned with immersion at 25 C, the test confirmed the effect
of the aggregate surface temperature only for porphyry aggregates (Table 8), where
adhesive failures prevail. For limestone aggregates, however, the better adhesive
bond with asphalt yielded purely cohesive or hybrid failures and therefore the
surface temperature had minor effects.

Table 8. Influence of surface temperature on pull-off strength after immersion at


25 C

Porphyry Aggregate Limestone Aggregate

Surface temperature Surface temperature


Binder type Binder type
Significant? p-value Significant? p-value
CRM-Elvaloy YES 0.003 CRM-Elvaloy NO 0.1333

FH-Elvaloy YES 0.008 FH-Elvaloy YES 0.0003

CRM-SBS YES 0.0002 CRM-SBS NO 0.1729

FH-SBS YES 0.0003 FH-SBS YES 0.0089

50/70 YES 0.0002 50/70 NO 0.1218

70/100 YES 0.001 70/100 YES 0.0004

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

Table 9. Influence of surface temperature on pull-off strength after immersion at


40C

Porphyry Aggregate Limestone Aggregate


Surface temperature Surface temperature
Binder type Binder type
Significant? p-value Significant? p-value
CRM-Elvaloy NO 0.2673 CRM-Elvaloy YES 0.0008

FH-Elvaloy YES 0.0014 FH-Elvaloy YES 0.0007

CRM-SBS NO 0.2386 CRM-SBS NO 0.7466


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FH-SBS NO 0.1297 FH-SBS NO 0.5525

50/70 NO 0.3508 50/70 NO 0.3964

70/100 NO 0.2215 70/100 NO 0.4923

4.3.5. Effect of water temperature


The water temperature during the conditioning phase, 25 C or 40 C, was an
important parameter to control the moisture damage. The importance of the
aggregate type was again emphasized.
With porphyry aggregates, immersion at 25 C yielded a significant reduction of
pull-off strength as the failure mechanism changed from cohesive to adhesive. With
limestone aggregate, this effect was less important.

Table 10. Effect of moisture on the pull-off strength after immersion at 25 C

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%

FH-SBS YES < 0.0001 19%

50/70 YES < 0.0001 35%

70/100 YES 0.0015 18%

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.

Table 11. Loss in pull-off strength due to the immersion in water at 40 C

Loss in pull-off strength (%) Loss in pull-off strength (%)


Binder type Binder type
Limestone Porphyry Limestone Porphyry

CRM-Elvaloy 36% 55% FH-SBS 28% 83%

FH-Elvaloy 26% 63% 50/70 69% 79%

CRM-SBS 34% 77% 70/100 37% 68%

4.3.6. Evaluation of the asphalt binders


The results of the PATTI tests showed that a comparison between asphalt
binders is possible only if taking into account the aggregate type. In other words, the
asphalt-aggregate interactions need to be considered. As shown in Table 11, the loss
in pull-off strength was lower for both modified binders (SBS and Elvaloy) than the
un-modified asphalts for the Limestone aggregates. For the Porphyry aggregates, on
the other hand, the FH-SBS binder showed higher loss (more water damage) than
the unmodified asphalts. It is also worth noting that the CRM based modified
binders (CRM-Elvaloy and CRM-SBS) show higher resistance to cohesion loss
(with Limestone) than the FH-Based modified binders. This trend suggests that there
are positive effects of higher asphaltene content on cohesion, while the modification
type effects on cohesion are somewhat negligible.
For the porphyry aggregate, where adhesive failures prevailed, a different effect
of modification is observed since in this case better results (less loss in strength)
were obtained with the Elvaloy modification.
30 Road Materials and Pavement Design. EATA 2010

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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