Construction and Building Materials 41 (2013) 216223

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Construction and Building Materials

journal homepage: www.elsevier.com/locate/conbuildmat

New design method of ne aggregates mixtures and automated method for analysis
of dynamic mechanical characterization data
Pedro Sousa a,, Emad Kassem a, Eyad Masad b, Dallas Little b
a
b

Texas A&M Transportation Institute, Texas A&M University, 3135 TAMU College Station, TX 77843-3135, United States
Zachry Department of Civil Engineering, Texas A&M University, 3135 TAMU College Station, TX 77843-3135, United States

h i g h l i g h t s
" The new design method results in easy to compact specimens with SGC.
" DMA samples are easy to core from the SGC specimens.
" New method based in current standard AASHTO procedures.
" Aggregate type had great impact on the moisture susceptibility of the asphalt mixtures.
" Developed software was used to analyze the DMA test data, calculate crack radius index.

a r t i c l e

i n f o

Article history:
Received 26 July 2011
Received in revised form 23 October 2012
Accepted 22 November 2012
Available online 9 January 2013
Keywords:
Fatigue cracking
Moisture damage
Asphalt mixtures
Dynamic Mechanical Analyzer (DMA)
Fine Aggregate Matrix (FAM)

a b s t r a c t
Studies have shown that Dynamic Mechanical Analyzer (DMA) is a good method to evaluate the resistance of the Fine Aggregate Matrix (FAM) portion of asphalt mixtures to cracking and moisture damage.
However, a systematic, simple method to design FAM that accurately represents the composition and
structure of that portion of the mixture needs to be developed. New procedure for preparing FAM specimens and software to analyze the data from the DMA and calculate fracture mechanics-based parameters were developed. The new specimen preparation method and software were successful in analyzing
the moisture susceptibility of FAM mixtures prepared using different materials.
2012 Elsevier Ltd. All rights reserved.

1. Introduction
Asphalt mixtures experience many distresses over their service
lives such as rutting, fatigue cracking, and moisture damage. Recently, several studies have successfully used the Dynamic
Mechanical Analyzer (DMA) to evaluate the resistance of the Fine
Aggregate Matrix (FAM) portion of asphalt mixtures to fatigue
cracking and moisture damage [17]. FAM is usually called asphalt
mastic, and it is a combination of an asphalt binder and the ne
portion of the aggregate gradation passing sieve No. 16
(1.19 mm). The DMA characterization of FAM was shown to be in
agreement with laboratory and eld performance of full mixtures
[2,3].
Earlier studies used a standard aggregate gradation and a xed
percentage of asphalt binder to prepare FAM samples irrespective
Corresponding author. Tel.: +1 979 845 8308; fax: +1 979 845 0278.
E-mail addresses: pedro.sousa203@gmail.com (P. Sousa), emasad@civil.tamu.
edu (E. Masad).
0950-0618/$ - see front matter 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.conbuildmat.2012.11.038

of the gradation of the aggregate or asphalt content of the full mixture [1,2]. The Superpave Gyratory Compactor (SGC) was used to
compact the FAM mixtures in laboratory. Small FAM specimens
(12 mm diameter by 50 mm height) were cored and cut out of
the SGC specimens (152.4 mm diameter by 85 mm height) [2].
The preparation method of FAM mixtures was later improved to
better estimate the binder content by estimating the lm thickness
coating each aggregate particle in the full mixture [46]. However,
this method yielded a high asphalt content that caused problems in
compacting the FAM specimens using the SGC. Therefore, it was
decided, based on practical laboratory experience, to use 70% of
the calculated FAM asphalt content [4,6]. In this paper, a method
for the preparation of FAM specimens is presented such that the
composition of FAM specimens accurately represents the aggregate gradation and asphalt content of the ne portion of the full
mixture.
The researchers at Texas A&M University have developed a
fracture mechanics-based approach for the analysis of DMA data
and characterization of the resistance of the FAM to fatigue and

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P. Sousa et al. / Construction and Building Materials 41 (2013) 216223

moisture damage [3,5,6,8]. This method requires input parameters

that describe the viscoelastic properties, adhesive bond energy,
and energy dissipation of the material. The use of this method requires detailed, time consuming data processing and calculations.
Therefore, it was deemed necessary to automate the analysis
method to increase the efcacy of DMA testing and analysis to
engineers in the characterization of asphalt mixtures.
This study was conducted to achieve the following primary
objectives,
 Develop a new procedure for preparing FAM samples in order to
describe the composition and structure of the ne portion of the
full mixture.
 Develop user-friendly software to analyze the DMA data and
calculate parameters that describe the FAM resistance to fatigue
cracking and moisture damage.
 Utilize the new specimen preparation method and software in
the analysis of FAM specimens that are composed of different
materials.
2. New design method of FAM mixtures
As discussed earlier, the design of FAM mixtures should be
based on the gradation and composition of the full asphalt mixtures of which they represent a crucial part. The FAM consists of
the ne portion of the mixture with aggregates passing sieve the
No. 16 sieve (1.19 mm). The proportioning of the ne aggregates
that comprise the FAM was kept the same as in the full mixture
aggregate gradation, but they were normalized with respect to
the largest sieve in the FAM (#16). This means that 100% of the
aggregate in the FAM passes sieve No.16, and the percent passing
the smaller sieves is calculated as in Eq. (1):

Percent passing siev e x in FAM

Mass of aggregate passing siev e x in full mixture

Mass of aggregate passing siev e #16 in full mixture
 100%

A comparison of FAM aggregate gradation and the corresponding

full mixture gradation is given in Fig. 1.
The new method for the determination of the binder content relies on experimentally separating the ne portion of the mixture
(passing sieve number 16) from the coarse portion and determining the asphalt content of the ne portion. This asphalt content
is then used to mix and compact FAM specimens in the SGC. The
new method takes advantage of the procedures described in AASHTO standards T 209 and T 308 for determining the theoretical maximum specic gravity and binder content in asphalt mixtures,

Table 1
Minimum sample sizes.
Minimum sample
size (g)

P37.5
19.0 or 25
612.5

4000
2500
1500

respectively [9,10]. The proposed procedure can be summarized

in the following steps:
 Prepare three loose samples of the full asphalt mixture. The
minimum mass for each sample is given in Table 1, as indicated
in AASHTO T 209 [9].
 Subject the samples to a 2 h conditioning period in an oven at
135 5 C following AASHTO T 209 procedure [9].
 Take the mixture out of the oven, and let it cool for approximately 30 min.
 Separate the mixture particles by hand as described in the
AASHTO T 209 procedure, which is used in determining the theoretical maximum specic gravity [9]. If the separation cannot
be achieved at room temperature, the asphalt mixture should
be placed in a at pan and warmed in an oven until it can be
separated by hand. Once particles are separated, spread them
on a smooth surface, and let it cool for 30 min.
Use a mechanical sieving machine to sieve the loose asphalt
mixture into different sizes (#4, #8 and #16). To help separating
the particles during sieving, 9.5 mm stainless steel balls were
placed in each sieve. Recommended amount for the steel balls
are 40, 30, and 20 corresponding to sieves numbers 4, 8, and 16,
respectively (Fig. 2a). The properties of steel ball are described in
the micro-deval test apparatus AASHTO T 327 [11]. The result
is four groups of material sizes:




Group 01: material retained on sieve #4,

Group 02: passing sieve #4 and retained on #8,
Group 03: passing sieve #8 and retained on #16, and
Group 04: passing sieve #16.
Dry each material group at a temperature of 110 C.
Place each material group in a pan, and record the mass of the
pan (WP) and the mass of the pan with each material group
(WMi) using a balance with a minimal precision of 0.1 g for
groups 1, 2 and 3 and minimal precision of 0.001 g for group
4. The subscript i refers to the group number (14).
 Place the pan with each material group in an ignition oven
apparatus to burn the asphalt (Fig. 3a). The ignition oven temperature was 427 C. The asphalt burning is considered complete after at least 10 min and when there is no change in
mass more than 0.01%. After the binder burning is completed,
remove the pan from the oven and place over a cooling plate
to rest for approximately 30 min (Fig. 3b).
 Record the mass of the pan with each of the groups (WAi).
 Calculate the binder content for each material group as indicated in Eq. (2):

Pbi

Fig. 1. Proportioning of aggregates in FAM.

Nominal maximum aggregate

size (mm)

W Mi  W Ai
 % where i 1 to 4
W Mi  W p

The binder content in group 4 (Pb4) is the asphalt content that

was used to prepare the FAM mixtures.
The FAM specimens are compacted in the SGC compactor. These
specimens were 100 mm in diameter and 85 mm in height. The
amount of materials needed to prepare one FAM specimen is about
1800 g. This specimen is compacted in the SGC until there was no

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P. Sousa et al. / Construction and Building Materials 41 (2013) 216223

Fig. 2. Sieving the mixture. (a) Set of sieves with steel balls and loose asphalt mixtures before sieving. (b) Mechanical sieving process.

Fig. 3. Ignition oven procedure. (a) Loose asphalt mixture before ignition oven. (b) The pan with residual materials after burning.

DMA Sample
Trimmed SGC
Samples

DMA Samples
SGC Samples

(a)

(b)

(c)

(d)

Fig. 4. Steps in FAM sample production. (a) SGC sample, (b) trimmed SGC sample and DMA samples, (c) DMA sample glued with, and (d) DMA device and the installation.

change in height with additional gyrations (Fig. 4a). These SGC

specimens are then trimmed to 50 mm in height (Fig. 4b). DMA
test samples with a diameter of 12.5 mm were cored out of the

SGC samples (Fig. 4b and c). Fig. 4d shows the DMA device and a
DMA sample during the test. The FAM mixtures evaluated in this
study had 2.53.5% air voids.

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P. Sousa et al. / Construction and Building Materials 41 (2013) 216223

Table 2
Mixtures composition details.
Mixture
label

Aggregate
passing
sieve #16 (%)

Filler passing sieve #200 (%)

In relation to the full mix

In relation to the FAM mix

A
B
C
D

26.0
27.0
30.8
26.1

6.14
5.1 (2% lime)
4.0 (1% lime)
2.75

23.6
18.9
13.0
10.5

Binder grade

Original mixture
binder content (%)

FAM binder
content (%)

Aggregate type

PG
PG
PG
PG

4.5
5.3
4.3
4.7

8.0
7.0
7.8
8.6

Limestone
Granite
Gravel
Limestone and gravel

7022
7028
6422
7622

2.1. Test materials

DGf dry DGa

Test materials used in this study were chosen to represent

aggregates that are used in the state of Texas. Four different mixtures were evaluated, and a summary of the mixtures, materials
compositions, and asphalt binders are given in Table 2.

DGf wet

3. Overview of fracture mechanics-based analysis of damage in

FAM
The fatigue life and moisture susceptibility of FAM mixtures are
evaluated by determining the amount of energy dissipated during
the application of cyclic fatigue loading of the DMA specimens. The
DMA test can be conducted in either the stress-controlled or
strain-controlled mode. In the strain-controlled mode, a constant
displacement is applied to the material at each cycle causing damage and a drop in the applied stress throughout the test. In stresscontrol, a constant stress level is applied to a specimen, which
causes incremental damage and an increase in the resulting strain
[8]. In this study, the researchers used the strain-controlled mode.
A fracture mechanics-based model has been successfully used
by Masad et al. [8] and Caro et al. [5] to analyze DMA test results.
The concept of this model is based on the original work of Schapery
[12] and Lytton et al. [13]. Lytton et al. [13] used the J-integral that
quanties the pseudo-energy release rate per unit crack area (JR) as
given in Eq. (3):

dr
AJ R n
dN

where r is the average crack radius in the sample, N is the number

of cycles, A and n are material constants and JR can be given as
shown in Eq. (4).
@W R
@N
J R @csa

@N

where csa is the crack specic area and WR is the dissipated pseudostrain energy. Previous work has shown that there is a linear relationships between WR and ln(N) for strain-controlled testing as
presented in Eq. (5) [8].

W R a b; lnN

From Eqs. (3)(5), it is possible to derive a crack size index as in Eq.

(6) [2,6]:


n 1=2n1

GR b
DRN 2n 1n1
N
4pG1 DGf

where DGf is the work of adhesion between the asphalt binder and
the aggregate at a given cycle. This index is constant for dry specimens. In the presence of moisture, the work of adhesion decreases
as the moisture reaches the aggregatebinder interface. For this reason, Eq. (7) is used to calculate the bond energy DGf in Eq. (6) [6].

jGN j a
DG
GR

where DGa is the adhesive bond energy between asphalt binder and
aggregate under dry conditions, and is calculated from surface energy measurements of the asphalt and aggregate [14]. jGN j is the dynamic modulus measured at cycle N of the DMA fatigue test and GR
is the reference modulus and is taken to be equal to the linear viscoelastic dynamic modulus [5,6].
The parameters G1 and n in Eq. (6) are the coefcients of the
power law function in Eq. (8) that describes the linear viscoelastic
relaxation as a function of time:

Gt G1 G1 tm

where n is given by the relation in Eq. (9) [7,15]:

N 1

1
m

4. Software development
A product of this research is software to analyze DMA test data
in the fashion described above. This software can be used by
researchers, engineers, or technicians to analyze the DMA test data
and thus to avoid having to deal with all of the complexities involved in the calculations. The software is capable of analyzing
data from both the stress- and strain controlled modes.
The programming language used in the software development
was C# (pronounced see sharp), which is conceived to work in
Microsofts .NET environment. Several reasons support the use of
C#. First, it is similar to C++ (which is used worldwide) and its object-oriented framework. It is also supported by an extensive library and resources both for computing and calculation, as well
as for visual resources. Second, it is very secure, providing a safe
execution environment. Third, the C# language has its inherent
interoperability with Microsoft Ofce products, which facilitates
the implementation of the calculation steps and makes the software more user-friendly [16].
The inputs for the software are as follows:
 DMA test result from the fatigue test which includes the
dynamic modulus and phase angle values as a function of different loading cycles; the fatigue test results are analyzed by the
software to determine the relationship in Eq. (5) and calculate
the parameter b.
 The adhesive bond energy, DGa , which is obtained from surface
energy measurements; the software includes a database of surface energy measurements, which can be used to specify the
materials and calculate DGa if the mixture to be tested was prepared from materials for which surface energy measurements
are available. If such data are not available, one will probably
be able to nd aggregates and binders in the software that are
sufciently similar to those used so that a reasonable approxi-

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Fig. 5. Comparison between MATLAB and software calculations for dry and wet conditions; Mixture D.

4.1. Software validation

The crack radius index for test specimens calculated using the
software was compared to the one calculated using MATLAB program. The software utilized Microsoft Excel to conduct the analysis. Good correlation was achieved as presented in Fig. 5. The
difference between both methods was less than 10%, which is
attributed to the differences in tting some of the relationships
(e.g. Eqs. (5) and (8)) to the data. Examples of the results are shown
in Fig. 5 for wet and dry specimens.
5. Binder content results

Fig. 6. Binder contents of different mixtures. Asphalt contents and error bars (one
standard deviation away from the average) for each fraction group of all four
mixtures.

Table 3
Measured binder content for different fractions and binder content of full and FAM
mixtures.
Fraction groups

1
2
3
4
Design value for full mixture
Design value for FAM

Binder content (%)

A

3.81
6.69
7.37
8.00
4.50
8.00

4.35
5.99
6.57
6.97
5.30
7.00

3.48
5.82
7.80
7.28
4.30
7.80

4.13
6.6
8.06
8.65
4.70
8.60

mation of surface energies, and hence bond strengths can be

determined. The software combines dynamic modulus values
at different loading cycles with DGa to obtain DGf using Eq. (7).
 DMA test results of the relaxation test. The software uses these
data to determine the relationship in Eqs. (8) and (9) and calculate G1 and n.
 Frequency and the testing mode (controlled strain or controlled
stress).
 The output of the software is the crack radius index (Eq. (6)) as a
function of loading cycles.

Fig. 6 shows the determined asphalt content in different groups

with error bars for the three samples of each mixture. The determined binder content for different replicates was consistent within
each group. The maximum standard deviation of the estimated
binder content was 0.34% among all groups and 0.24% within
group 04 (FAM mixture). As expected, the small aggregates required more binder to coat the particles compared to the coarser
aggregates. This is due to the high surface area of the small aggregate particles. Table 3 shows the measured binder content for different sizes, design asphalt binder in the full mixture, and binder
content used to produce FAM mixtures. It should be noted that
group 4 of Mixture C had less binder content than Group 3 in contrast to all other mixtures. The researchers conducted sieve analysis for all materials after the ignition oven. They found that Group 3
of Mixture C had a considerable amount of ne materials from
Group 4 (passing # 16) after the ignition oven. Large part of Group
4 materials was sticking to Group 3 materials of Mixture C. The
researchers believed that this affected the determined binder content in Groups 3 and 4 of Mixture C. This issue would be avoided by
increasing the time of sieving. For the limitation of the materials
from Mixture C, the researchers were not able to repeat the test
using longer sieving time, and they decided to consider the binder
content of Group 3 instead of Group 4 for Mixture C.
6. Dynamic mechanical analysis of ne aggregate mixtures
The DMA samples were tested in dry and wet conditions. The
wet conditions were achieved by submerging DMA specimens in
distilled water under a vacuum of 3.38 kPa absolute pressure
(736.6 mm Hg partial pressure) for 20 min. The DMA device that
was used in this study had a maximum torque of 0.2 N m, and thus
this test was conducted at 30 C as some of the produced DMA

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P. Sousa et al. / Construction and Building Materials 41 (2013) 216223

Table 4
Parameters for the crack radius index fracture-based model.
GR = GLVE (Pa)

G1 (Pa)

DGf (J/m2)

392.58
346.53

9.08E+08
9.24E+08

1.31E+08
2.34E+08

0.423
0.381

3.327
3.623

0.097

Dry
Wet

412.13
419.15

5.43E+08
6.95E+08

6.85E+07
1.03E+08

0.389
0.403

3.568
3.479

0.109

Dry
Wet

419.14
1047.26

8.45E+08
6.93E+08

1.43E+08
2.65E+08

0.336
0.289

3.98
4.461

0.127

Dry
Wet

1576.25
2130.01

1.08E+09
8.32E+08

2.76E+08
5.03E+08

0.297
0.382

4.363
3.618

0.092

Mixture

Condition

Dry
Wet

b (J)

(a)

(c)

(b)

(d)

Fig. 7. Crack radius indexes of the four mixtures described in Table 4.

samples were stiff and the DMA was not able to apply the required
torque at room temperature. Recently, the researchers have acquired a new DMA with a torque limit of 5.2 N m, which is high enough to test any DMA samples regardless of the binder content.
In this study, the researchers used the strain-controlled mode to
test the specimens. First, a constant shear strain of 0.0065% was applied to the test samples for 10 min. The test data were used to calculate the relaxation modulus (G1) and material constant (m) as
described in Eq. (8). Following the relaxation test, an oscillatory
test at low strain amplitude of 0.0065% and a frequency of 10 Hz
was applied for 2 min to characterize the other viscoelastic properties (modulus, G and phase angle, d). Then, a fatigue test was conducted at high strain amplitude of 0.35% and a frequency of 10 Hz.
The test data were used to determine the pseudostrain dissipated
energy and calculate the parameter b as given in Eq. (5). All data
were analyzed using the software developed in this study. Table 4
summarizes the average values of the parameters for each mixture

needed to calculate the crack radius index in Eq. (6) in both dry and
wet conditions.
The results produced by the software are plotted in Fig. 7 for the
four mixtures described in Table 4. The mixtures varied in their
binder grades; therefore, it was decided to compare the performance of these mixtures based on the ratio DRwet/DRdry rather than
on the value DRdry or DRwet. The mixtures varied in their points of
failure; however, for comparison purposes it was decided to plot
the results up to 30,000 cycles which was the shortest life among
all mixtures. Mixture C had the highest DRwet/DRdry value which
is attributed to the siliceous nature of the gravel aggregate used
in this mixture. Mixture D, which consisted of limestone and gravel, performed much better than Mixture A which included gravel
only. Mixture D was modied to include anti-strip liquid (Mixture
DAS) and lime (Mixture DL). The lime was added with a percentage of 1% by weight of aggregates in replacement of the nes. The
results from these two mixtures are shown in Fig. 8. The data are

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P. Sousa et al. / Construction and Building Materials 41 (2013) 216223

(a)

(b)

(c)

Fig. 8. Crack radius index and ratio. Mixture D, (a) unmodied, (b) modied with lime (DL), and (c) modied with anti-strip (DAS).

plotted to 100,000 which was the smallest fatigue life among these
three mixtures. The DMA test conrms that the presence of lime
enhances the resistance to moisture susceptibility. It is interesting
to note that the use of the anti-strip in this particular mixture lead
to a drop in the resistance to moisture damage.

7. Conclusions
In this study, a standard test procedure for preparing FAM specimens that represent the composition and structure of the ne portion of the asphalt mixtures was developed. In addition the authors
developed user-friendly software that was easy to use and capable
of analyzing the DMA data and presenting the results in simple formats. Such software can be used to analyze both stress- and straincontrolled DMA tests. The following are the main ndings of this
study:

 The new design method for preparing FAM mixtures always

produced specimens that were easy to compact using the
Superpave Gyratory Compactor (SGC) and core in the
laboratory.
 The new method was consistent in measuring the asphalt content in the ne portion of the mixture.
 Aggregate type had great impact on the moisture susceptibility
of the asphalt mixtures. It was shown that the FAM mixtures
that were prepared using limestone had better resistance to
moisture damage than the ones prepared using gravel.
 The developed software was used to analyze the DMA test data
and present the results in simple formats. The crack radius
index calculated using the software was very close to the value
calculated manually.
 The ease of use of the software is expected to promote further
implementation of the DMA in the characterization of FAM to
evaluate the resistance of asphalt mixtures to moisture damage
and fatigue cracking.

P. Sousa et al. / Construction and Building Materials 41 (2013) 216223

 The new method for preparing FAM mixtures will be implemented in a proposed AASHTO procedure for characterization
of FAM.

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