Chapter 3

1.0 Methodology

1.1 Intoduction

This chapter discusses several tests that were conducted in achieving the objectives of the study. All tests
were carried out at University Tun Hussein Onn Malaysia Transportation Laboratories. Study will be
carried out by using experimental methods to evaluate the performance of Natural Rubber (Latex) and its
suitability in road pavement precisely in hot mix asphalt. The sample testing on Latex as modifier in
bitumen is carried out through the bitumen tests.

In this study, the laboratory works can be divided into two stages with bitumen of 80-100 PEN are used in
this study. The first stage was a mix between bitumen with Natural rubber (latex) separately and then
mixing percentage of latex with bitumen. Testing on these specimens have to be carried out is Dynamic
Shear Rheometer (DSR) in order to ensure it performs well on the superpave specifications. All test are
carried out to test whether the modified binders was appropriate. The amount of latex modifier added to
the mixes was expressed in percentage (1%,3%,5%) of the total weight of bitumen.

For second stage, a lot of specimens will prepared from bitumen mix with latex according different
percentage between them. The objective of superpave mix design is to determine the optimum Latex and
bitumen with the aggregate to ensure the mixture air voids.
1.2 operation framework

Start

Sample preparation
and test

Bitumen Aggregate

Variation of (NR) Gradation of

aggregate
0,1%,3%,5%
Variation of Nr

1%,3%,5%

Blending the
aggregate

PAV Test RTFO test

DSR test Mix design by

superpave

Opt. mixture composition

(1%,3%,5%) NR

Performance test (dynamic creep and wheel tracking test)

 1.3 sample preparation (1st stage)

For stage one, normal bitumen 80-100 PEN will be prepared at 160°C meanwhile Natural rubber is added
to modified bitumen. The blending of modifiers and bitumen using manual mixer take around 30 minutes
to mix with NR.

The numbers of sample required are:

a) 1 sample of normal bitumen (DSR Test);

b) 3 samples of normal bitumen and 3 sample for each percentage of NR by weight of bitumen for
modified bitumen (DSR Test);

Bitumen %NR
300g 1 3 5

1.3.1 Binder selection and acquisition

The selection of binders was according to the superpave binder specification (ASTM D6373) requirement
several test are uses in this specification. The binders are selected on the basis of the climate and traffic in
which they are intended to service. The location of road was selection for this study is Malaysia.
Therefore, the DSR test was selected to use in the performance grade method to characterize and to
determining the rheological properties of the asphalt binder. The asphalt binders are tested in conditions
that simulate its critical stages during service, such as:

 During transportation, handing and storage-original binder is tested.

 During mix production and construction-simulated by short term aging the original binder a
rolling thin film oven (RTFO).
 After 5 to 10 years of service- simulated by long term aging the binder in the rolling thin film
oven test plus the pressure aging vessel (PAV). In the PAV, the RTFO residue is exposed to high
air pressure and temperature for 20 hours to simulate the effect of long-term pavement aging.
1.3.1.1 Rolling thin film oven (RTFO)

The rolling thin film oven produce is to simulate the short term aging that occurs in the asphalt during
production of asphalt concrete. In the RTFO method (ASTM D2872) will as next operation
procedure.

Test equipment:

a) RTFO apparatus as shown in figure 3.2;

b) 8 bottles
c) Air compressor

Procedure:

a) Switch on the RTFO power and set temperature at 163°C;

b) Dry the bottles to place the asphalt specimens inside it up 35±0.10 gm/bottle as figure 3.3 (a) and
(b).
c) Switch on air compressor
d) Put the bottles inside RTFO as figure 3.4
e) Press the red alarm button
f) The specimens need inside the RTFO in this condition for 85 minutes
g) After the time test finished and the bottle coating, poured the specimens as figure 3.5 to the
container to prepare it to DSR test.
1.3.1.2 Pressure-Aging Vessel (PAV)

The PAV as illustrated in figure 3.6 is designed to simulate the oxidative aging that occurs in asphalt
binders during pavement service. Residue from this process may be used to estimate the physical or
chemical properties of an asphalt binder after 5 to 10 years in the field. The PAV consists of
temperature control chamber, and pressure, sample pan and rack and temperature controlling and
measuring device as shown in figure 3.6. The test of PAV in this study according to (ASTM D6521)
will be as follow:

Test equipment:
To prepare of the PAV samples, each samples should weight 50g residue from approximately two
RTFO bottles tested are transferred to individual PAV pan.

Procedure

i. Open gas cylinder valve;

ii. Turned on the temperature chamber and placed the vessel in the chamber
iii. Placed the sample pan in the sample rack and;
iv. Remove the vessel from the oven when the temperature reached 100°C and put the sample
rack in the hot vessel;
v. To avoid excessive loss of vessel heat the lid has been installed and the screw is tightened;
vi. Press age button. Aging light is red and wait for 25 minutes and the pressure will
automatically increase to 2 MPa and after that the aging light is become green and test run
for 20 hours.
vii. After 20 hours, the pressure will automatically reduce to 0 and complete light become green
with and temperature remains at 100°C.
viii. Before opening the vessel lid the pressure reading is less than 0.07MPa;
ix. Removed the pan from the sample holder and placed in an oven at 163°C for 15-30 minutes
to remove the entrapped air from the samples.
x. Transferred the sample to a container to storage for further testing DSR test and switch off
PAV and gas cylinder valve.

1.3.1.3 Dynamic shear Rheometer (DSR)

Researchers used the DSR as figure 3.7 to characterize the viscous and elastic behavior of asphalt
binders at medium to high service temperature. The DSR measures a specimen’s complex shear
modulus (G*) and phase angle (δ) of asphalt binders at desired temperature and frequency of loading.
Complex shear modules and phase angle are calculated automatically by the rheometer computer
software.
 Complex shear modulus is a measure of the total resistance of material to deformation when
repeatedly sheared, and the phase angle is lag between the applied shear stress and the resulting shear
strain. The phase angle for perfectly elastic material is 0 degrees and for viscous fluid is 90 degrees.
The specified DSR oscillation rate of 10rad/sec (1.59Hz) is meant to simulate the shearing action
corresponding to a traffic speed about 55 mph (90km/h). Consists of the DSR apparatus are:

a) Computer
b) Two parallel metal plates;
c) An environmental chamber;
d) Loading device; and
e) Control and data acquisition

The basic procedure for DSR as follow:

i. Heat the asphalt binder from which test specimens (RTFO-PAV) are to until the binder is
sufficiently fluid to pour the test specimens in the container.
ii. Select the testing temperature according to the asphalt binder testing schedule
iii. Make the specimen with 1mm thickness and bring the oscillating (top) plate to place the
specimens under it
iv. Fix the plate in its place
v. Run the test with the temperatures that needed to finish it.

This procedure is doing for three types of testing (unaged or virgin binder – RTFO residue _PAV
residue). This will be conduct three tests on the samples and examined on DSR test to determining the
rheological properties of the asphalt binder.
 1.4 sample preparation (for 2nd stage)

For stage two, Normal bitumen 80-100 PEN will be prepared to use with the different percentage but the
temperature will be different to the mixture between the NR, bitumen and aggregate. Next steps show the
superpave mix design process.

1.4.1 Aggregate

The aggregate used in this research within superpave condition and are consists of coarse and fine
aggregate. Laboratory test that will be conducted on aggregate are:

a) Sieve analysis of coarse and fine aggregate.

b) Specific gravity of coarse aggregate
c) Specific gravity of fine aggregate.

a) Sieve analysis of coarse and fine aggregate.

Sieve analysis is the process of separating aggregate into different sizes through a series of sieves
progressively smaller opening to determine the grading and distribution of aggregate for superpave
mixture, the procedure is based on (SP-2).

Apparatus:

a) Oven
b) Sieves
c) Mechanical sieve shaker
d) Balance

Procedure:

I. Dried the samples to constant weight at temperature of 110±5°C

 II. Nested the sieves in order of decreasing size of opening from top to bottom and the samples were
places on the top sieve.
III. Turn on the shaker to agitate the sieve for a sufficient period of time.
IV. Weight the percentage passing versus sieve size on the sieve chart along with its gradation limits.
V. Check whether the aggregate size distribution meet the specified mix gradation.

1.4.1.1 Aggregate gradation

The percentage of aggregate required for every sieve size were determined according to superpave
(SP-2/1996). Then the mass retained were calculated using the percent passing for every sample size.

B) specific gravity and water absorption of coarse aggregate

The procedure covers the specific gravity test of coarse aggregate and will determine the value of
bulk and apparent specific gravity and absorption of coarse aggregate after 24 hours soaking. The
equipment and procedure for determining the specific gravity and absorption of this test were outlined
in ASTM C 127.

Apparatus:

i. Balance
ii. Water tank
iii. Sieve
iv. Sample container
Procedure:

i. The aggregate were mixed and washed so as to clean it from dust and weighed approximately
quantity needed, 1kg.
ii. The sample was soaked in water for 24hours.
iii. After 24 hours, the sample was weighed together with water and the mass is recorded.
iv. Dried the sample with a damp towel until it was saturated surface dry and weighed again and the
mass of the sample was recorded.
v. Dried the sample in an oven for 24hours at 110±5°C and let it cool before weighing for the third
time and the mass of the sample was recorded.
vi. Specific gravity was calculated as follows:

𝐶
Bulk Sp. Gr = 𝐵−𝐴

𝐶
Apparent Sp. Gr = 𝐶−𝐴

𝐵−𝐶
Absorption (%) = 𝐶
∗ 100

With:

A= weight of saturated samples in water,g

B= weight of saturated samples surface-dry samples in air, g

C= Weight of oven-dry samples in air, g

C) Specific gravity and water absorption of fine aggregate

The specific gravity test will determined the value of bulk and apparent specific gravity of fine aggregate.
The equipment and procedure for determining the specific gravity and absorption of fine aggregate were
according to ASTM C 128.

Apparatus:

i. Balance with 0.1g accuracy

ii. Pycnometer
iii. Mold in the form of a frustum of a cone with dimensions as follow:
90±3mm inside diameter at the bottom, 40±3mm inside diameter at the top, and 75±3mm in
height.
iv. Tamper having a flat circular face 25±3mm in diameter and weighing 340±15 g.

Procedure:

I. 500g weight of sample was placed in the container and 30g(6% of the sample) of water was
mixed together in order to get a saturated surface-dry condition for 24 hours.
II. Partially the pycnometer was partially fill with water.
III. Immediately the pcynometer was introduced with the approximately 500g of saturated surface dry
sample prepared.
IV. The additional of water was filled to approximately 90% of capacity.
V. The pcynometer was rolled, inverted and agitated to eliminate all the bubbles.
VI. The total weight of pycnometer, sample and water were recorded as ‘C’ to the nearest 0.1g.
VII. Removed the sample from the pycnometer and dried constant weight at temperature of 110±5°C
VIII. Cooled the sample in air at room temperature
IX. The weight was recorded to the nearest 0.1g as ‘A’
X. Recorded the weight of the pycnometer filled with water as ‘B’
XI. Specific gravity was calculated as follows:
 𝐴
Bulk Sp. Gr = 𝐵+𝑆−𝐶

𝐴
Apparent Sp. Gr = 𝐵+𝐴−𝐶

𝑆−𝐴
Absorption (%) = ∗ 100
𝐴

With:

A = Weight of oven-dry sample in air, g

B = Weight of pycnometer filled with water, g

C = weight of pycnometer filled with aggregate and water, g

S = Saturated surface-dry weight of the sample, g

 1.4.2 Dynamic creep test

Creep is defined as the continuous time dependent deformation under constant stress or load. Creep test
data characterize the permanent deformation properties of asphalt mixtures. Creep compliance and mix
stiffness are good parameters for relative mix stability and the excepted rut depth or permanent
deformation.

The dynamic creep test is a test that applied a repeated pulsed uniaxial stress/load to an asphalt (or other
materials) specimen and measures the resultingdeformation in the same axis and/or radial axis linear
variable displacement transformers (LVDTs). Test can also be conducted under confined conditions using
a standard triaxial pressure cell or the IPC global developed rapid triaxial Tester (RaTT). The stress/load
applied to the specimen is feedback controlled allowing the operator to select a loading wave shape
(havesine or square pulse), the pulse width duration, the rest period before the application of the next
pulse, the deviator of stress/load to be applied so that the vertical loading shaft does not lift off the test
specimen during the rest period. Prior to testing preload stress/load can also be programmed into the
testing sequence. For controlled temperature testing, the specimen’s skin and core temperature are
estimated by transducers inserted in a dummy specimen and located near the specimen under test.

Test was carried out on Universal Test Machine (UTM), with feedback control hydraulic tester and with a
temperature controlled environment chamber. As the loading and measuring device, data were collected
and analyzed by automated testing system.

The dynamic creep test software conforms to the following international test standards and test methods.

a) Australian: AS 2891.12.1
b) British : DD 226
c) European : prEN 12697 – 25a
d) European : prEN 12697 – 25b
e) US : NCHRP 9-19 Superpave models draft test method W2 (Unconfined)
f) US : NCHRP 9-19 Superpave models draft test method W2 (Confined)
Procedure:

a) As illustrated in figure 3.12 seated the specimens one by one between two plates with the
constant temperature skin 40°C and known height for each specimens.
b) Separate jigs are provided for either 100mm or 150mm diameter specimens which are mounted
vertically in the loading frame. The jigs comprise an upper and lower loading platen which
distribute the load evenly to the ends of the specimen. The lower jigs has a locating slot that
mates with a pin fitted to the base of the loading frame to ensure proper registration directly
under the loading ram of the actuator.
c) With the lower platen located on the base of the loading frame, prepare the ends of the specimen
as required (this may simply involve the application of a graphite grease, or use an aluminium foil
layer) than centrally mount the specimen on the lower jig platen.
d) Place the upper platen centrally on the specimen. Now lower the loading shaft and ensure that the
ball end seats correctly in the tapered hole of the top platen. Note: that it may be necessary to
adjust the height of the loading frame cross arm to ensure that, not only do the specimen and jig
fit, but that sufficient actuator travel remains to allow for specimen deformation during the test.
e) Vertical axial displacement is measured with LVDT transducers. These are typically calibrated
over the range from zero to 5mm. the transducers are mounted on support rods attached to the
axial loading jig base plate, with the probes end bearing on the upper loading platen surface.
Ensure that the transducers operate over their calibrated operating range using the Transducers
levels display.

1.4.3 wheel tracking test

Laboratory wheel-tracking devices (Figure 1) are used to run simulative tests that measure
HMA qualities by rolling a small loaded wheel device repeatedly across a prepared HMA
specimen. Performance of the test specimen is then correlated to actual in-service pavement
performance. Laboratory wheel-tracking devices can be used to make rutting, fatigue, moisture
susceptibility and stripping predictions. Some of these devices are relatively new and some
have been used for upwards of 15 years like the French Rutting Tester (FRT).

In general, these wheel tracking devices have potential for rut and other measurements but the
individual user must be careful to establish laboratory conditions (e.g., load, number of wheel
passes, temperature) that produce consistent and accurate correlations with field performance.

Procedure:
1) Prepare either 6 cylindrical or 3 beam test samples (Figure 8). Laboratory compacted cylindrical
samples should be compacted to 4 percent air voids and be 3 inches (75 mm) tall. Laboratory
compacted beam samples should be compacted to 5 percent air voids and be 3 inches (75 mm)
tall. Field core samples should have a 6 inch (150 mm) diameter and either be 3 inches (75 mm)
tall or be augmented with plaster-of-paris to produce a 3 inch (75 mm) tall sample.
2) Determine the bulk specific gravity (Gmb), maximum specific gravity (Gmm) and air void
content (Va) of each sample.
3) Set the test temperature at the high temperature specification of the PG binder used.
4) Preheat the samples in the APA or a calibrated oven for 6 hours.
5) Set the hose pressure and load cylinder pressure to the desired levels. Typically, 120 psi (827
kPa) is used for the hose and 120 lb (534 N) is used for the load.
6) Stabilize the test chamber at the desired temperature.
7) Insert the test samples into the chamber.
8) Apply 25 cycles to seat the samples.
9) Open the chamber doors, unlock and unseat the sample, and place the rut depth measurement
template over the sample.
10) Zero the gauge and take initial rut depth readings. Repeat this step for each set of cylinders of
beams in the APA.
11) Push the sample holding tray in, close the APA doors and allow 10 minutes for the test
temperature to stabilize.
12) Set the APA counter to 8,000 cycles.
13) Start the APA loading.
14) At the end of 8,000 cycles, repeat step 10 to get the final rut depth measurement