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Estimating the Thermal Conductivity of Asphalt Binders
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Carlos J. Obando, Ph.D. (c).1 and Kamil E. Kaloush, Ph.D., P.E.2
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1School of Sustainable Engineering and the Built Environment, Arizona State University, P.O.
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Box 873005, Tempe, Arizona 85287-3005; e-mail: cobandog@asu.edu
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2School of Sustainable Engineering and the Built Environment, Arizona State University, P.O.
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Box 873005, Tempe, Arizona 85287-3005; e-mail: kamil.kaloush@asu.edu
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Published in: Journal of Testing and Evaluation (ASTM)
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DOI: 10.1520/JTE20210208
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ABSTRACT
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Nowadays, there is a common worldwide interest in environmental issues and pavements.
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How to save energy and mitigate the urban heat island (UHI) effect are topics that are drawing the
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attention of different researches and industrial organizations. In road infrastructure, one of the
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important properties addressing environmental and UHI aspects of pavements is the determination
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of the thermal conductivity. Asphalt concrete represents the third most widely used resource in the
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world, with asphalt-paved roads being its principal usage. One of the most important components
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of asphalt concrete is bitumen. Bitumen is a viscoelastic material susceptible to temperature
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changes. The determination of the bitumen´s thermal conductivity becomes very important in
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understanding and improving its thermal performance. There are very few test methods and
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equipment to measure thermal conductivity of bitumen (asphalt binders). Some are expensive and
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require special equipment and instrumentation. This study developed and validated a simplified
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testing technique to measure thermal conductivity of asphalt binders. This test is a steady state-
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based method to estimate the thermal conductivity of asphalt binders using cylindrical samples
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poured into a silicon mold. The method was validated using material of known thermal
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conductivity. Eighteen samples of different binder grades were tested, and the test results were
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repeatable and within known thermal conductivity values. Sensitivity analysis and accuracy of the
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proposed method were validated modifying the asphalt binder with a material with a very low
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thermal conductivity. This method to estimate thermal conductivity of bitumen samples was found
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to provide an affordable alternative test procedure with good accuracy and precision.
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Keywords: Thermal conductivity, bitumen, steady-state method, heat transfer rate
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INTRODUCTION
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There is a common worldwide interest in environmental issues and pavements. One aspect
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is the mitigation of the urban heat island (UHI) effect. In road infrastructure, one of the important
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materials properties in addressing the UHI of pavements is the determination of the thermal
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conductivity. The thermal conductivity is a physical property that is also related to the performance
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of the materials, which implies the energy transfer rate or heat transfer rate (Q) that occur when
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bodies in contact have different temperatures1.
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Heat can be transferred from one point to another by three different processes: conduction,
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convection and radiation2. Conduction can occur in solids, and in liquids when there is no
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macroscopic movement. Convection occurs when liquids are in movement, and radiation occurs
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in the vacuum or air. These modes of heat transfer are governed by different laws, Fourier, Newton,
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and Stefan-Boltzmann, respectively
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This document addresses the conduction phenomenon of bitumen. In conduction, heat is
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transmitted through a material medium and there is no transport of matter. The rate at which heat
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is transferred through the material (dQ/dt) is represented by the letter Q and is called the heat flow
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3
rate. Empirically, the heat flow rate is proportional to the cross-sectional area (A) to the direction
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of the flow, to the temperature difference on both sides of the material (∆T), and inversely
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proportional to the distance traveled from the place at the highest temperature (∆x) [3]. That is:
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(1)
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To achieve the equality of the previous expression, a constant k is added, which is the
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thermal conductivity, the intrinsic ability of a material to transfer or conduct heat3 4.
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(2)
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The conduction into a cylindrical geometry, introduces the Equation 35 6.
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(3)
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Where:
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Q: heat flow rate (W=joule/s)
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A: the cross-sectional area (m2)
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ΔT: the temperature gradient (oC)
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Δx: the thickness (m)
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k: the thermal conductivity (W/moK)
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t: time (s)
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h: length/height of the sample (m)
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4
r1: inner radius (m)
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r2: outer radius (m)
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Thermal conductivity is inherent to each material and expresses the ability of a given
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material to conduct heat3. Thermal conductivity can be affected by moisture, ambient temperature,
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and the density of the material. If moisture, temperature, and density are increased, the thermal
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conductivity rises too, so thermal conductivity is not constant1.
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The exactitude of different methods for calculating thermal conductivity is extensively
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debated in several fields. In addition, the wide range of thermal characteristics of different
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materials generated several methods for the estimation of thermal conductivity7.
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Along the last two decades, the accuracy and the understanding of the principles of heat
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transfer have been improved for several materials. These techniques present different ranges of
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thermal conductivity even for the same material, different accuracy, temperature ranges, and
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specimen type8.
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Although there are many methods to estimate thermal conductivity, there are few for
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specific materials like bitumen, or asphalt binder. There are two basic methods. The first one is a
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group of steady‐state methods, and the second one is called the transient or a group of non‐steady‐
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state methods7 9. The implementation of each method depends on the characteristic of the materials.
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All methods are based on electrical analogy and on the essential laws of heat conduction. Steady‐
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state methods are mathematically simpler8, while transient heat transfer methods are efficient to
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determine thermal diffusivity. However, steady‐state methods are known as the most accurate for
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testing dry materials10.
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The steady‐state technique is related to an equilibrium state, then, these methods consider
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the data to do the calculations when a material reaches a constant temperature. As a disadvantage,
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to reach a steady temperature takes a long time1. In addition, these methods involve expensive
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equipment and difficult experimental set-up installation. Nonetheless, steady-state methods are the
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most accurate and the main measurement methods. The non‐steady‐state or transient methods take
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measurements during the heating progression. These techniques estimate thermal conductivity
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using transient sensors. The time needed in these methods is relatively quick, which is the most
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important advantage over the steady‐state systems11. Table 1 shows a summary of the principal
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characteristics of the various methods.
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In the Civil Engineering field, asphalt concrete represents the third most widely used
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material in the world, with asphalt-paved roads being its principal usage. One of the most important
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components of asphalt concrete is bitumen, a residue of oil distillation processes. Bitumen is a
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highly susceptible viscoelastic material to temperature changes. This can be brittle as glass at low
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temperature and flow like oil at high temperatures12. From this conception, the determination of
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thermal conductivity of the bitumen becomes very important to understand and improve its thermal
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performance.
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Analytical models in different studies have been used to calculate the thermal conductivity.
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However, the accuracy of each model and technique is constricted by the physical properties and
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other factors of each material to test. Therefore, quantity and modeling of thermal conductivity are
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complex and need high precision. The approaches and the models used to study thermal behavior
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of materials must be clearly defined8.
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Table 1. Summary of methods used for the determination of the thermal conductivity8
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Method
Usage
Uncertainly
Estimation
Range of
Temperature
Advantages
Disadvantages
Steady‐ state methods
Guarded hot
plate
Solids, insulator
materials
2% –5%
−93°C – 127°C
High level of accuracy
Long measurement time,
low conductivity
materials, large
specimen size
Heat‐flow meter
Rocks, polymers,
insulations, plastics,
glasses, ceramics, some
metals
3% –10%
(normal), 0.5% –
2% (axial) and
3% –15% (radial)
−100°C–200°C
(normal), -183°C–
126°C (axial heat
flow), and 25°C –
2326°C (radial heat
flow)
Easy operation and
construction
Relative measurement,
uncertainly
Cylinder
Metals
2%
-269°C – 727°C
Simultaneous
estimation of electrical
conductivity, and
temperature range
Long measurement time
Pipe method
Calcium, silicates, solids,
refractory fiber blankets
and minerals
3% –20%
20°C – 2500°C
Good temperature range
Long measurement time,
specimen set up
Comparative
Plastics, metals, ceramics
10% –20%
20°C – 1300°C
Simple construction and
operation
Relative measurement,
uncertainly
Direct heating
Tubes of electrical
conductors, metals,
wires, rods
2% –10%
127°C – 2727°C
Easy and fast
measurements,
simultaneous estimation
of electrical
conductivity
Limited to electrically
conducting materials
Transient Methods
Hot disk (TPS
technique)
Solids, powders, liquids,
pastes
--
247°C – 927°C
Diverse thermal
properties
simultaneously, and
accuracy
Conducting or insulating
material
Hot wire
Hot strip
Hot wire: Solids, liquids,
glasses, plastics,
granules, powders
Hot strip: Ceramics,
glasses, foods
1% –10 % hot
wire
5% –15% hot
strip
20°C –2 000°C, −40–
1600°C for hot wire
and −50°C to 500°C
for hot strip, 25°C –
1527°C for hot wire
Fast, accuracy, and,
good temperature range
Only for low
conductivity materials
Photothermal
(PT)
Photoacoustic
Thin films, solids,
liquids, gases
1%–10 % for PT
−50°C – 1500°C, and
-73°C – 527°C for PT
Operational for liquids,
gases, and thin films
Unknown accuracy,
Nonstandard
Laser flash
Polymer, ceramics,
solids, liquids, powders,
metals
1.5% –5 %
−373°C – 3027°C
Good temperature
range, accuracy at high
temperature, small
specimens, fast
Expensive, not for
insulation materials
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Based on the unique characteristics of bituminous materials, and the need to know their
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thermal properties for better understanding the potential improvement when using various
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modification techniques, this document presents an alternative method for determining the thermal
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conductivity of bitumen, while addressing issues like cost and accuracy.
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EXPERIMENTAL APPROACH
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Calibration
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The determination of the thermal conductivity of bitumen samples using the method
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described in this document was first used on material of known characteristics and thermal
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conductivity. The calibration sample used was acrylic glass (Plexiglas V045i), which has a known
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thermal conductivity range between 0.17W/moK and 0.20W/moK13 14; in confirmation, and
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following the method developed at The National Center of Excellence for SMART Innovations at
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ASU15, the thermal conductivity of this material was estimated as 0.1852W/moK.
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As it was explained above, thermal conductivity is related to the heat transfer rate, which
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is central in the estimation of thermal conductivity in this method. Due to the unique characteristics
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of the bitumen/asphaltic binder, the medium to transfer the heat was chosen as distilled water in
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no macroscopic movement. Then, the temperature transfer from the outside to the sample is
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realized using non-turbulent, distilled water. At the liquid-solid interface, the main mechanisms
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contributing to heat transfer are convection and conduction. However, the present work restricts
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the domain study to the sole solid sample. This assumption is sustained by the fact that the bitumen
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is considered as a solid. Therefore, it is possible to restrict the heat transfer rate (Q) calculation to
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a conduction-driven mechanism only, using Equation (3).
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The heat flow rate is independent of radial location but varies depending on the temperature
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of the water; therefore, it was necessary to calibrate the model measuring the heat flow rate at
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several temperature points. This calibration method compares different water temperatures and the
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resulting heat flow rate, knowing the thermal conductivity, and the acrylic-sample’s geometrical
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features.
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To determine the heat flow rate, we need to measure the two final steady temperatures in
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the system. In this approach, the outer temperature is the water temperature being controlled by
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the water bath, and the inner temperature is the one in the center of the acrylic sample. Note that
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the “system” includes all instrumentation features like water bath, thermocouple types and
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accuracy, and thermometers, which are described next.
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Instrumentation
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To avoid the interference of air currents that could alter the temperature readings and make
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it more difficult reaching the steady state temperatures, the experimental setup was employed
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inside a chamber conditioned at 25oC. To control the water temperature, a water bath (Thermo
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Scientific, 180 Series, Model: Precision) was used. For temperature measurements, J type thermal
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couples (-40 to 510 oC) were used, and a software LabVIEW 8.6 with a DAQ system were used to
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record the temperature changes along with time. To check the accuracy of the temperature
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readings, a high precision thermometer (Precision RTD Handheld Data Logger Thermometer) was
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used.
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The acrylic samples used to calibrate the model were cylindrical shaped. The samples are
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40mm in diameter (r2, the outer radius is then 19mm), and 25mm in height (h), with a hole of 2mm
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diameter (r1=1mm, which is the inner radius) in the center of the top circular face, extending to the
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middle of the sample. Figure 1 shows the cylinder’s geometry.
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Figure 1. Acrylic sample characteristics
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To measure the thermal conductivity in steady state using a conduction method, it is
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necessary to ensure that the heat flow goes only in one direction. A balsa wooden platform was
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used to place the samples inside the water bath. This setup is needed to avoid the water outer
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temperature affecting the inner temperature in the center of the acrylic cylinder. An isolator foam
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was used on the top of the acrylic sample, and a high vacuum grease silicone on the bottom. This
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particular grease has sealing ability and at the same time excellent resistance to water.
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Additionally, because the relative high specific heat capacity, 2900 J/kgK16, a very low thermal
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conductivity, 0.045W/moK17, of the balsa wood, the very low power in the system (e.g. 0.09W at
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47oC), and the short time of the test (2 hours), it is considered that no significant heat enters from
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the bottom of the sample. The samples were submerged into the water bath taking care that the
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level of water goes near the edge of the top circular face. For temperatures above 50oC, it is
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recommended to cover partially the water bath to avoid water evaporation. Figure 2 shows the
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complete setup.
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Figure 2. Complete set-up of the calibration test
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The final data needed to calculate Q are the steady-state temperatures. Figure 3 shows
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examples of the temperature change recorded for various samples versus time. The steady-state
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temperatures are those when the inner (center of the sample) and outer (water) temperatures reach
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a unchanging condition.
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Figure 3. Temperature vs. Time
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After certain time period, the temperatures get to the steady state. Note that the time needed
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to get to the steady state may vary; however, for this setup the usual time was 1.5 hours. Once the
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steady-state temperatures are reached, it is recommended to continue recording readings for at
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least 30 minutes and calculate the average value.
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From Equation 3, knowing the geometrical characteristics of the specimen (refer Figure 1),
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the thermal conductivity constant of the acrylic material (k), and the difference between inner and
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outer temperatures (ΔT), it is possible to calculate the heat flow rate for each temperature. Figure
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4 shows Q for different water temperatures ranging between 31oC and 82oC.
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Figure 4. Heat flow rate (Q) as a function of the temperature (oC)
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Note that the acrylic material was used to estimate the heat flow rate of the system, which
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has a thermal conductivity of 0.185W/moK. Equation 4 represents the results of the calibration
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process to find Q as a function of water temperature; it can be used subsequently to calculate the
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thermal conductivity (k) .
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(4)
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12
Where:
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Q: heat flow rate (W=joule/s)
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T1: the outer temperature (water temperature) (oC)
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The estimation of ¨Q¨ is an important step to determine the thermal conductivity of any test
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samples of interest using Equation 3. It depends on the thermal conductivity of the acrylic
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calibration sample being used. Therefore, the constant number 0.0153 in the exponential Equation
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4 may change. In addition, the exponent part constant 0.0412 in the equation would remain the
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same if the system components being used are kept unchanged. This is because the exponent
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constant in the equation is dependent on the system configuration (e.g. water bath characteristics).
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Thermal conductivity of bitumen/asphalt binder
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To employ the above test procedure, it is needed to produce asphalt-binder samples with
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similar dimensions to the acrylic cylinders. Therefore, special molds are needed to be made and
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used to pour in them the hot asphalt binder. The material used to create the mold was a commercial
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product that consists of two liquid substances. These substances need to be mixed in a specific
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proportion to get the raw silicone material. This silicone material can support temperatures above
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300oC. Figure 5 shows the silicone container / mold used to produce the asphalt binder samples
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for testing.
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Figure 5. Silicon mold used for asphalt binder samples production and testing (“h” corresponds to the
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inner depth of the mold).
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The use of silicone molds is very convenient due to their flexibility. Once the hot binder is
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poured in the mold and cooled down, a 2mm diameter hole is drilled in the center from the top to
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the middle of the cylinder height, similar to the acrylic cylinder test procedure described earlier.
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The hole in the center is made using a heated metallic rod or a screwdriver, both with appropriate
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diameters. As the air inside the samples can affect thermal conductivity, it is important to pour the
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material in the mold as hot as possible and leave it to cool down slowly undisturbed at room
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temperature. Before drilling or removing the samples from the mold, it is recommended to place
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the asphalt binder samples inside a freezer for 20 minutes at -10 oC. Figure 6 shows how the binder
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samples look like inside the silicone mold, and Figure 7 shows how those binder samples look like
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when removed from the containers.
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Figure 6. Asphalt binder sample inside the silicone mold
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Figure 7. Asphalt binder samples ready to test
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Thermocouples are placed in the center hole, and the samples are placed on wooden
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platform. The isolator foam is placed on top, and high vacuum grease silicone on the bottom of
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the circular face of each sample. The grease helps the samples get locked on the wooden platform,
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isolating water at the bottom, and avoiding samples getting stuck. Figure 8 shows the final setup
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of the test before adding the foam on top. Note that the level of the water is just at the edge of the
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samples.
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Figure 8. Setup of the thermal conductivity test on binders
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Based on known thermal susceptibility of the asphalt binders, it is recommended to perform
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the test between 28oC and 40oC to avoid the softening of the samples. The temperature of the water
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would vary depending on the type of binder being evaluated. For softer binders such us PG58-22,
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and PG64-16, the recommended maximum test temperature is 28oC, which is about 15oC below
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their softening point measured with the ring and ball method (ASTM E28 – 67). For stiffer binders
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such as PG76-22, the recommended maximum test temperature is 33oC. Binders modified with
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polymers can be tested up to 40oC.
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This method could be implemented using any type of water-bath following the calibration
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step described earlier in this document. In earlier experiments, the authors had also good success
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in using type K thermocouples with an automatic USB output thermometer, and/or manually
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registering temperatures with time. Care in selecting, manipulating and calibrating the
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thermocouples and water-bath will provide repeatable and accurate results.
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This method can be used to calculate the thermal conductivity of any material with
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impermeable properties, so the water in the system, which controls the outer temperature, cannot
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get to the center of the sample where the inner temperature is taken.
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RESULTS OF THE IMPLEMENTATION
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Eighteen samples of different virgin binders (PG58-22, PG64-16 and PG76-22) provided
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by HollyFrontier in Arizona, were tested using this developed method. Binders PG58-22 and
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PG64-16 are unmodified bitumen used for hot mix asphalt, emulsion production or further
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modification for higher temperature paving grades; whereas binder PG76-22 is a modified asphalt
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cement used for hot mix asphalt. The softest of these asphalt binders is PG58-22 and the stiffest is
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PG76-2218. Soft binders are more susceptible to temperatures changes and flow more at high
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temperature than stiff binders. It is also noted that lower ability of the binders to conduct heat
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(lower k) means better thermal resistance.
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To get the heat flow rate (Q) for the three asphalt binders, Equation 4 of the base calibration
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model were used. Once Q is found, thermal conductivity is calculated based on the Equation 3
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solving for Thermal Conductivity (k). As it was mentioned before, the whole system is employed
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inside a chamber setup at 25oC, and the resulting thermal conductivity is estimated under this
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condition. Table 2 and Figure 9 show all the test results presenting the coefficient of variance
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(COV) and the standard error respectively. The average test results for each binder grade produced
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repeatable outcomes that are similar to known thermal conductivity values as shown below; the
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coefficient of variation was also under 10% for each binder. While the average thermal
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conductivity between the binder grades are statistically the same, there seem to be a trend of having
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17
slightly lower thermal conductivity for stiffer binders. This result is rational as one would expect
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a PG76-22 binder with a polymer modification should have lower thermal conductivity compared
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to a conventional softer binder. Figure 9 present the results showing the standard error.
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Table 2. Thermal conductivity of different binders
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Binder Type
Sample No.
Sample's
Height
h (m)
Sample's
radius
r2 (m)
Sample's
radius
r1 (m)
Outer Temp.
(water) T1 (C)
Flow Rate Q
(W)
From Eq 4.
Sample's
Inner Temp.
T2 (C)
k (W/moK)
From Eq 3.
Av. k
(W/moK)
COV
Binder PG58-22
1
0.0250
0.019
0.010
31.37
0.05572
30.23
0.200
0.209
0.08
2
0.0250
0.019
0.010
31.15
0.05521
30.16
0.227
3
0.0250
0.019
0.010
31.15
0.05521
29.89
0.179
4
0.0250
0.019
0.010
31.20
0.05533
30.18
0.222
5
0.0250
0.019
0.010
31.00
0.05487
29.95
0.214
6
0.0250
0.019
0.010
31.40
0.05578
30.32
0.211
Binder PG64-16
7
0.0250
0.019
0.010
31.37
0.05572
30.16
0.188
0.204
0.07
8
0.0250
0.019
0.010
31.15
0.05521
30.1
0.210
9
0.0250
0.019
0.010
31.15
0.05521
29.9
0.183
10
0.0250
0.019
0.010
31.20
0.05533
30.15
0.215
11
0.0250
0.019
0.010
31.00
0.05487
29.98
0.220
12
0.0250
0.019
0.010
31.40
0.05578
30.31
0.209
Binder PG76-22
13
0.0250
0.019
0.010
31.37
0.05572
30.25
0.203
0.198
0.08
14
0.0250
0.019
0.010
31.15
0.05521
29.9
0.177
15
0.0250
0.019
0.010
31.15
0.05521
29.9
0.177
16
0.0250
0.019
0.010
31.20
0.05533
30.10
0.206
17
0.0250
0.019
0.010
31.00
0.05487
29.95
0.214
18
0.0250
0.019
0.010
31.40
0.05578
30.31
0.209
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439
440
441
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Figure 9. Average thermal conductivity of binder with the standard error
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Salt remains
18
Thermal conductivity of asphalt binders can range between 0.17W/moK and 0.28W/moK
446
19 20. From Table 2, it is possible to see that k varies between 0.23W/moK and 0.18W/moK (note
447
that in the calculation, Celsius degrees are transformed to Kelvin). Thermal conductivity results of
448
the different binders could confirm the better thermal resistance of the binder PG76-22, one of the
449
reasons to choose hard binders for a better asphalt pavement performance in hot climates.
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To better demonstrate the capability of the developed test method in capturing a different
452
thermal conductivity value for modified binders, the PG76-22 binder was modified with 5% Enova
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Aerogel. Aerogel is a material with extremely low thermal conductivity of about 0.012 (W/ moK)21
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22. The effect of the Aerogel’s low thermal conductivity when added to binder was studied using
455
the proposed method. For sample preparation, once the PG76-22 binder reached 165oC in the oven,
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5% of Enova Aerogel by weight of binder was added and blended manually using a wooden stick
457
for about 1 minute. The Aerogel modified binder along with a control were tested using the
458
proposed method and the thermal conductivity results obtained are shown in Table 3.
459
460
461
Table 3. Thermal conductivity of unaged binder PG76-22 with different methods
462
Binder Type
Sample No.
Sample's
Height
h (m)
Sample's
radius
r2 (m)
Sample's
radius
r1 (m)
Outer
Temp.
(water) T1
(C)
Flow
Rate Q
(W)
From
Eq 4.
Sample's
Inner
Temp.
T2 (C)
k (W/moK)
From Eq 3.
Average k
(W/moK)
COV
Control
1
0.0250
0.019
0.010
33.91
0.06185
32.71
0.211
0.199
0.06
2
0.0250
0.019
0.010
33.91
0.06185
32.63
0.198
3
0.0250
0.019
0.010
33.91
0.06185
32.56
0.188
5% Aerogel
1
0.0250
0.019
0.010
33.91
0.06185
32.25
0.153
0.166
0.08
2
0.0250
0.019
0.010
33.91
0.06185
32.49
0.179
3
0.0250
0.019
0.010
33.91
0.06185
32.38
0.166
463
19
The results supported the capability of the proposed test method in capturing lower thermal
464
conductivity values, as expected, for the Aerogel modified binder. The precision for the modified
465
samples was slightly lower, most likely due to the difficulty in uniformly distributing the Aerogel
466
particles in the binder samples.
467
468
469
CONCLUDING REMARKS
470
The determination of thermal conductivity of the asphalt binders is very important in the
471
understanding and improvement of its thermal performance. There are very few test methods and
472
equipment to measure thermal conductivity of asphalt binders. Some of those are expensive and
473
require special equipment and instrumentation. This study developed and validated a simplified
474
alternative testing technique to measure thermal conductivity of asphalt binders. The determination
475
of the thermal conductivity of bitumen samples using the method described was validated on
476
material of known thermal conductivity. In addition, eighteen samples of different binder grades
477
were tested using the developed method. The average test results were repeatable and within
478
known thermal conductivity values reported in the literature; the coefficient of variation between
479
the various samples were in the 7 to 8% range. Additionally, the sensitivity and capability of the
480
proposed method to capture lower thermal conductivity values were proven by using an Aerogel
481
modified binder. This method to estimate thermal conductivity of bitumen samples was found to
482
provide an affordable alternative test procedure with good accuracy and precision.
483
484
DATA AVAILABILITY STATEMENT
485
The data that support the findings of this study are available from the corresponding author,
486
Carlos Obando, upon request.
487
20
ACKNOWLEDGMENTS
488
The authors would like to thank the Global Kaiteki Center at Arizona State University for
489
the funding support. Additional support was provided by The National Center of Excellence for
490
SMART Innovations and the Advanced Pavement Laboratory at ASU. Based on the Program
491
Colombia Cientifica focuses/challenges related to Sustainable Energy, this work serves as a tool
492
for Sustainable Construction and a Cleaner Transportation development. The authors would like
493
to acknowledge the invaluable support provided by the Colombian Program Colombia Cientifica
494
and the Scholarship Fulbright - Pasaporte a la Ciencia.
495
496
497
AUTHOR CONTRIBUTIONS
498
In this article, Carlos Obando performed all laboratory experiments, designed the
499
experimental plan, analysis of the results, and participated in the development of the research topic.
500
Kamil E. Kaloush provided an overall guidance for the research conduct, interpretation of the test
501
results, and editing the manuscript.
502
503
504
505
506
507
508
509
510
21
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