Investigation of Rheological Effects of Waxes On Different Bitumen Sources

Road Materials and Pavement Design
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Investigation of rheological effects of waxes on

different bitumen sources
Julide Oner & Burak Sengoz
To cite this article: Julide Oner & Burak Sengoz (2017) Investigation of rheological effects of
waxes on different bitumen sources, Road Materials and Pavement Design, 18:6, 1269-1287, DOI:
10.1080/14680629.2016.1209123
To link to this article: https://doi.org/10.1080/14680629.2016.1209123
Published online: 26 Jul 2016.
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Download by: [Siddaganga Institute of Technology] Date: 23 November 2017, At: 03:25
Road Materials and Pavement Design, 2017
Vol. 18, No. 6, 1269–1287, https://doi.org/10.1080/14680629.2016.1209123
Investigation of rheological effects of waxes on different bitumen sources

Julide Onera∗ and Burak Sengoz b
a Facultyof Engineering, Department of Civil Engineering, Usak University, Usak, Turkey; b Faculty of
Engineering, Department of Civil Engineering, Dokuz Eylul University, Izmir, Turkey
Downloaded by [Siddaganga Institute of Technology] at 03:25 23 November 2017
(Received 5 February 2016; accepted 28 June 2016 )
Wax in bitumen has been referred to as petroleum wax and is obtained from refining of paraf-
finic crude oils. The effects of wax on bitumen properties depend on the following factors: the
source, chemical composition and rheology of the bitumen as well as the content, type, com-
position and crystallisation of the wax. There is a lack of literature reviews related to the effect
of waxes on the rheology and properties of bitumen. The scope of this study is to evaluate the
rheological properties of waxy bitumens obtained from different sources. Following the deter-
mination of wax contents by differential scanning calorimetry (DSC) and EN 12606-1, waxy
bitumen properties were evaluated using conventional methods, rotational viscosity, dynamic
shear rheometer (DSR) and bending beam rheometer (BBR) tests. The intermediate and high-
temperature performances levels of bitumen were also determined according to the Superpave
system by a DSR test performed on aged and unaged samples. Rutting performance of bitu-
mens has been evaluated using zero shear viscosity (ZSV) and multiple stress creep recovery
(MSCR) tests.
Keywords: wax; differential scanning calorimetry; bending beam rheometer; dynamic shear
rheometer; zero shear viscosity; multiple stress creep recovery
1. Introduction
Bitumen is an adhesive material used as an agent in flexible pavements as well as in other areas of
application, such as water proofing, flooring and joint materials. Bitumen is a very complex mate-
rial including hydrocarbon molecules with small amounts of heteroatoms consisting of sulphur,
nitrogen and oxygen, and gradually liquefies when heated (Redelius & Soenen, 2015).
Almost all bitumen is obtained from crude oil by a refining process but only certain crude
oils contain good-quality bitumen for asphalt pavement (Lyne, Wallqvist, & Birgisson, 2013).
Naphthenic-base crude oils often give a large amount of bitumen that may be in good quality,
while paraffinic crude oils may give bitumen of good quality or may yield bitumen that is not
suitable for asphalt pavement (Edwards & Redelius, 2003).
The term “wax” is generally defined as an organic compound that is solid at ambient temper-
ature and melts at higher temperatures, producing a low viscosity liquid (Soenen et al., 2013).
Natural wax is a part of practically all bitumens and may affect the rheology of bitumen in
different ways (Canestrari, Graziani, Pannunzio, & Bahia, 2013).
The definition of bitumen wax has been formulated to facilitate the distinction between harm-
ful wax and less harmful or non-harmful ones. Waxes in bitumen are divided into two general
categories such as paraffin wax (macro-crystalline) and micro-crystalline wax (Edwards, 2009).
*Corresponding author. Email: julide.oner@usak.edu.tr
© 2016 Informa UK Limited, trading as Taylor & Francis Group

1270 J. Oner and B. Sengoz
Paraffin wax, also known as macro-crystalline wax, crystallises in large flat plates or needles. It
refers to the group of n-alkanes with few or no branches (C20 –C40 ) (Soenen et al., 2013). The
melting point of macro-crystalline paraffin waxes is around 50–70°C (Lu, Langton, Olofsson, &
Redelius, 2005; Lu, & Redelius, 2007). On the other hand, micro-crystalline wax is collected
in the bitumen fraction after the distillation process and mainly consists of naphthenes and iso-
paraffins as well as crystallises as small microscopic needles. A micro-crystalline petroleum wax
is characterised also by a less distinct melting area and its high average molecular weight pro-
ducing higher viscosity compared to macro-crystalline paraffin wax (Das, Kringos, Wallqvist, &
Birgisson, 2013; Musser, & Kilpatrick, 1998).
Definitions of wax concepts have varied over the years and sometimes have been contradictory
(Edwards, 2009; Redelius & Soenen, 2015). The effect of waxes depends on chemical composi-
tion (source) and rheological behaviour of the bitumen as well as content and crystallinity of the
wax. Consequently, many bitumen specifications include requirements concerning wax content.
It has been reported that wax content in bitumen should not exceed 3% and the wax content is
limited to 2.2% in Europe by the EN 12606-1 method (Wong & Li, 2009).
Based on literature, the high content of wax affects the properties of bitumen in different ways.
The low melting point of wax decreases resistance of asphalt mixtures against rutting at high tem-
peratures, and the crystallisation of wax causes cracking at low temperatures (Lu & Redelius,
2006). Physical hardening, poor ductility and poor bitumen adhesion can be listed as the out-
comes caused by the high content of wax (Edwards & Redelius, 2003). The performance grade
of bitumen at high temperature may decrease with melting of wax.
Somewhat contradictorily, the benefits of wax in bitumen have been reported, such as
improved low-temperature properties and lower handling temperatures (for better compaction)
(Redelius, Lu, & Isacsson, 2002). The Strategic Highway Research Programme recommends
some additional rheological and chemical tests on unaged, short-term-aged and long-term-aged
bitumen to evaluate the exact definition of the wax concept (Petersen et al., 1994).
This paper evaluates the rheological behaviour of waxy bitumens obtained from four differ-
ent sources. Following the determination of wax contents by differential scanning calorimetry
(DSC) and EN 12606-1, the detailed properties of bitumen samples have been evaluated using
dynamic shear rheometer (DSR) and conventional methods. The upper critical temperatures used
in the Superpave performance grading (PG) system have been determined for each bitumen sam-
ple using G*/sin δ results gained from the DSR test. The effects of loading and temperature
on the performance of the waxy bitumen samples have been evaluated by low- (0.01 Hz) and
high-frequency (10 Hz) loadings at five different temperatures (40–80°C). Fatigue properties of
bitumen have been evaluated by the fatigue factor at intermediate temperatures. Besides, the
bending beam rheometer (BBR) test has also been conducted to investigate the lower critical
temperatures of bitumens. Rutting performance of bitumens has also been evaluated using zero
shear viscosity (ZSV) and multiple stress creep recovery (MSCR) tests performed in creep mode.
2. Experimental methods
2.1. Materials
Seven bitumens from four different sources (Turkey, Iraq, Russia and Turkmenistan) were used
in this study. The bitumen samples are identified as Bit-TR; Bit-I, Bit-R and Bit-TU, respectively.
The general description of samples together with penetration grades are depicted in Table 1.
Since the bitumens are originated from different sources, their wax contents are different.
Bit-TR1 and Bit-I were manufactured from crude oil deposited in the east part of Turkey and
the north part of Iraq, respectively. Russia (Bit-R1, Bit-R2 and Bit-R3) bitumens, Bit-TR2 and
Road Materials and Pavement Design 1271
Table 1. The general description of samples.
Source of bitumens Abbreviation Sample no. Penetration grades
Turkey Bit-TR Bit-TR1 50/70

Bit-TR2 40/60
Iraq Bit-I Bit-I 70/100
Russia Bit-R Bit-R1 60/90
Bit-R2 60/90
Bit-R3 70/100
Turkmenistan Bit-TU Bit-TU 50/70
Bit-TU were produced by the blending of crude oil from various sources by a manufacturer in
Western Siberia, Middle Eastern countries and Turkmenistan, respectively. Besides, a limited
amount of air blowing was used to manufacture Bit-R1 during the refining process.
2.2. Test methods

2.2.1. Determination of the paraffin wax content based on European Standard Method EN
12606-1
The European Standard EN 12606-1 is based on DIN 52015, a German method that is performed
for determining the paraffin wax content of bitumen samples (Baldino et al., 2012; European
Standard EN 12606-1, 2007). The system includes a distilling system, an electric cooler, a
thermo-regulator and refrigeration compressor.
The test procedure is performed in two portions for each 25-g bitumen sample. The distillate
from bitumen is obtained by a specified distillation process. The distillation unit consists of a
distillation flask, a laboratory burner and Erlenmeyer flask used as distillation receiver. The dis-
tillation takes place at very high temperatures (up to over 500°C) at which cracking of molecules
may occur (Lu & Redelius, 2006). In the second portion of the test procedure, the waxy distillate
is dissolved in ether/ethanol (50/50, V/V) solvent and crystallised at − 20o C. The crystallised
wax is obtained by filtration (European Standard EN 12606-1, 2007).
2.2.2. Differential scanning calorimetry (DSC)

The crystallisation or melting of waxes in bitumen causes energy change. Both heating and cool-
ing cycles can be used to investigate the presence of wax fraction in bitumen. The exothermic
and endothermic effects during the cooling and heating scan generally represent the wax crys-
tallisation and wax melting, respectively. The DSC method has been utilised to register thermal
effects of waxes in bitumen through the cooling–heating cycles (ASTM D4419-90, 2015).
In this study, thermal characterisation was performed using DSC; Perkin Elmer-Diamond.
Approximately 15 mg of bitumen is placed in an aluminium pan and sealed under nitrogen
atmosphere. The bitumen sample is heated to + 120°C and then cooled at 7°C/min to − 50°C,
followed by heating to + 120°C at the same rate. DSC procedure is also used to determine wax
content in bitumen. The DSC wax content of bitumen is calculated from an endothermic peak
during the heating scan. For the calculation of percentage of wax in the bitumen, a constant melt-
ing enthalpy value of 121 J/g is used as a reference (Lu, Kalman, & Redelius, 2008). A typical
DSC diagram is presented in Figure 1.
Glass transition temperature, wax crystallisation starting temperature and melting out tem-
perature are also determined by the results gained from the DSC test. The glass transition
temperature (Tg ), defined as the half-vitrification temperature, is the midpoint of the transition
Figure 1. A typical DSC diagram through the cooling–heating cycles.
region (Edwards, Tasdemir, & Isacsson, 2006). The glass transition temperature obtained from
the heating scan is more repeatable and easier to obtain in comparison to the cooling scan. From
DSC, bitumen exhibits a kind of phase transition on cooling from high temperature and heating
from low temperature. The first transition has been considered as crystallisation starting temper-
ature (Tic ) in the cooling cycle. Besides, the new phase transition has occurred during the heating
cycle. There is an endothermic reaction which is interpreted as melting of the wax. Wax melting
out temperature that is defined as Tfm is the end point of wax melting in bitumen.
2.2.3. Conventional bitumen tests

In order to characterise the properties of different sources of bitumen, conventional tests such
as: penetration test (ASTM D5-06), softening point test (ASTM D36-06), ductility test (ASTM
D113-86), Fraass breaking point test (EN 12593), viscosity at 60o C (ASTM D4402-06) and
rolling thin film oven test (RTFOT) (ASTM D2872-12) as well as penetration, softening point,
viscosity at 60°C and ductility after RTFOT were performed (ASTM D5-06, 2006; ASTM D36-
06, 2006; ASTM D113-86, 1994; EN 12593, 2007; ASTM D4402-06, 2002; ASTM D2872-12,
2012).
In addition, the temperature susceptibility of the bitumen samples has been calculated in terms
of Penetration Index (PI) using the results obtained from penetration and softening point tests
(Whiteoak & Read, 2003).
The effect of viscosity on workability of bitumen is very important. Brookfield Viscometer
was employed at 135°C and 165°C to determine the viscosity of the bitumen samples (ASTM
D4402-06, 2002).
The reduction in the hardening of bitumen during storing, transportation and mixing depends
on careful control of bitumen temperature. The hardening factor is a measure of how sensitive
viscosity of bitumen is to aging. Obviously, bitumens having low hardening rates are desired. The
viscosity tests were performed on unaged and aged bitumen samples at 60°C when the material
is very nearly Newtonian. The ratio of the dynamic viscosity after RTFOT to dynamic viscosity
before aging at 60°C has been determined as hardening factor (ASTM D4402-06, 2002; Ruan,
Davison, & Glover, 2003).
2.2.4. BBR test

Creep test with BBR was carried out based on the ASTM D6648-01 standard test method
(ASTM D6648-01, 2001). BBR performs flexural tests, providing a measure of stiffness related
to bitumen at low temperatures. Before the test is performed, bitumen samples are subjected to
short-term and long-term aging procedures. Two parameters of bitumen samples are calculated
by engineering beam theory under a constant creep load. The first parameter is creep stiffness
(S), which is a measure of resistance to constant loading. The second parameter is the creep rate
(m), which is a value of how bitumen stiffness changes as load is applied.
A bitumen sample beam (125 mm in length, 12.5 mm in width and 6.25 mm in thickness)
was submerged into a constant temperature bath for 1 h. A constant load of 100 g was applied
to the midpoint of the bitumen beam which was supported at the ends. The deflection was then
measured continuously. Creep stiffness and creep rate of bitumens were evaluated at a loading
time of 60 s. Creep stiffness must not exceed 300 MPa and m-value must be at least 0.3 for a
qualified low-temperature cracking resistance.
2.2.5. Rheological test methods

The DSR is used to describe the viscous and elastic behaviour of bitumen at medium-to-high tem-
peratures. This characterisation is used in the Superpave PG asphalt bitumen specification. The
basic DSR test uses a thin bitumen sample sandwiched between two circular plates. The lower
plate is fixed while the upper plate oscillates back and forth across the sample at 10 rad/s (1.59
Hz) (or any other set frequency) to create a shearing action. DSR tests are conducted on unaged,
RTFOT-aged and pressure aging vessel (PAV)-aged bitumen samples. During the preparation
of aged bitumen, short-term aging procedure is achieved by RTFOT to simulate aging during
construction (ASTM D2872-12, 2012). The bitumen in a rolling glass bottle is heated in an oven
for 85 min at 163°C. Long-term aging, which simulates field aging during the first 5–10 years
of service, is achieved by further aging of the bitumen using the PAV. Residue from RTFOT is
placed in the PAV chamber and aged for 20 h under an air pressure of 2.1 MPa and an aging
temperature at 100°C (ASTM D6521-05, 2005).
The DSR measures a specimen’s complex shear modulus (G*) and phase angle (δ). The com-
plex shear modulus (G*) can be considered the sample’s total resistance to deformation when
repeatedly sheared, while the phase angle (δ) is the lag between the applied shear stress and the
resulting shear strain. G* and δ are used as predictors of rutting and fatigue behaviours. Early in
pavement life rutting is the main concern, while later in pavement life fatigue cracking becomes
the major concern. G*/sin δ is described as a rutting-indicating parameter and G*.sin δ as a
fatigue-cracking-indicating factor (Asphalt Institute, 2003).
The Superpave® specification parameter, G*/sin δ, was identified as the term to be used
for high-temperature PG of paving asphalts in rating of the bitumen samples for their rutting
resistance.
ZSV is the viscosity measured in shear deformation at a shear rate approaching zero. This
parameter is an indicator for rutting-related bitumen characteristics. It has been observed by
researchers in recent years that the rutting parameter G*/sin δ is not very effective or failed
to predict the rutting performance of bitumen (De Visscher, Soenen, Vanelstraete, & Redelius,
2004). The determination of ZSV in this study is performed by the application of creep test using
DSR. Static creep is defined as the slow deformation of a material measured under constant
stress. In the static creep test, a fixed shear stress is applied to the sample and the resultant strain
is monitored for a predetermined amount of time. If the stress is applied for a sufficiently long
duration of time, the deformation rate in the bitumen reaches a constant value, which corresponds
to the steady state flow of the bitumen. The viscosity of the bitumen at this stage is known as the
steady-state viscosity or the ZSV (Gungor & Saglik, 2012). All bitumen samples were short-term
aged using a RTFOT procedure. The ZSV of the samples have been predicted by application of
creep test at 60°C (CEN/TS 15325, 2008). The test geometry for the creep tests consisted of
25-mm parallel plates and the gap between the plates was 1 mm. The stress level was 10 Pa for
bitumen samples and each creep test was continued for 30 min.
Since the actual change of strain will be dependent upon the applied stress, it is usual to
mention about the compliance rather than the strain (Lu & Redelius, 2007). The compliance is
defined simply as the ratio of the strain to the applied stress and is denoted by the letter (J )
(Baldino et al., 2012). According to the theoretical assumptions of this method, the ZSV of a
material is represented by the inverse of the average slope that curve J (t) is assuming during the
last minutes (e.g. 15 min) of the test according to the following equation:
ZSV = t/J = 900/(Jf − J15 ) [Pa.s], (1)
where J 15 represents the compliance expressed in Pa−1 , measured 15 min before the load is no
longer applied, J f is the compliance expressed in Pa−1 , measured at the end of the 30 min and 900
is the time interval between the two measurements expressed in seconds (Laukkanen, Pellinen,
& Makowska, 2013).
Developments led to the performance of the multiple stress creep and recovery (MSCR)
test (Dubois, Mehta, & Nolan, 2014). The MSCR test was run on RTFOT-aged samples in
accordance to ASTM D7405-08 using the DSR (ASTM D7405-08, 2008). The ASTM standard
procedure establishes the use of two stress levels (0.1 and 3.2 kPa), 1-s creep time, 9-s recovery
time and 10 creep-recovery cycles at each stress level. Anton Paar DSR with its parallel-plate
geometry loading device and a control and data acquisition system were utilised for conducting
the MSCR test in the present study. Specimens were tested using 25-mm parallel plates and with
1 mm gap setting at temperature of 60°C and at a stress of 100 and 3200 Pa. Percents of recov-
erable and non-recoverable components of creep compliance were determined at the end of 10
cycles.
3. Results and discussions

3.1. Determination of wax content in bitumens through EN 12606-1 and DSC
The wax content is calculated by the following formula based on the European Standard Method
EN 12606-1. Wax content is calculated as:
m1 ∗ mw
P= ∗ 100 (2)
mb ∗ m2
where P (m%) is the wax content, mb (g) is the mass of specimen, m1 (g) is the total mass of
distillated oil, m2 (g) is the mass of distillated oil for wax extraction and mw (g) is the mass of
wax extracted (European Standard EN 12606-1, 2007).
The crystallisation or melting of waxes in bitumen involves energy change. This can be easily
determined by DSC. The results of the EN 12606-1 and DSC measurements are summarised in
Table 2 in terms of wax content, crystallisation starting temperature, wax melted out temperature
and glass transition temperature.
Table 2. DSC and EN 12606-1 analysis of bitumens.
Bitumen Bit-TR1 Bit-TR2 Bit-I Bit-TU Bit-R1 Bit-R2 Bit-R3
Sources Turkey Turkey Iraq Turkmenistan Russia Russia Russia

Wax content by EN 0.8 2.70 1.12 4.22 2.0 2.1 2.3
12606-1 (%)
Wax content by DSC (%) 2.61 3.52 3.27 7.74 4.81 3.93 4.04
Parameters Crystallisation starting 39.11 45.93 37.85 58.36 50.22 47.95 55.40
obtained temperature – Tic by
from DSC DSC (°C)
Melting out temperature – 65.97 84 86.42 62.08 80 65 83
Tfm by DSC (°C)
Glass transition temper- − 7.05 − 15.16 − 15.78 − 20.15 − 16.08 − 21.65 − 20.56
ature – Tg by DSC
(°C)
As indicated in Table 2, bitumen samples from different sources exhibit different wax contents
based on DSC and EN 12606-1 methods. It is clearly seen that the EN 12606-1 method gives
much lower values in wax content as compared with DSC. It is believed that the high temperature
(up to over 500°C) in the distillation step in the EN 12606-1 method may destroy the molecular
structure of waxes (thermal cracking). The resulting smaller paraffin molecules could be soluble
in ether/ethanol and these molecules do not crystallise in the solvent at the specified low tem-
perature ( − 20°C), yielding lower apparent wax content. These might be the reasons for the low
wax contents determined by the EN 12606-1 method. The difference in wax content between
DSC and EN 12606-1 may also be due to the wax solubility in bitumen providing a dissimilar
crystallisation/melting response in DSC. In fact, all available methods used for determining wax
content in bitumen only demonstrate relative results. Correlation between the EN 12606-1 and
DSC methods is presented in Figure 2. Although both DSC and EN 12606-1 methods are basi-
cally very different, they exhibit a reasonably good correlation with a regression coefficient (R2 )
Figure 2. Correlation between the EN 12606-1 and DSC methods.

of 0.78. The bitumen sample from Turkmenistan (Bit-TU) contains a large amount of wax com-
pared to other bitumen samples according to EN 12606-1 and DSC methods. However, Bit-TR1
from Turkey has the lowest amount of wax.
DSC has been widely applied to characterise the thermodynamics properties of bituminous
materials. In a cooling cycle, crystallisation occurs at different temperatures which are inter-
preted as wax crystallisation starting temperature (Tic ). The transition continues down to the
glass transition temperatures. In a heating cycle, there is an endothermic reaction which is inter-
preted as melting of the wax. Wax melting out temperatures of bitumens are defined as Tfm . The
temperature at which all wax is completely melted is considerably higher than the start of crys-
tallisation. This is due to the super cooling effect of the cooling cycle. Effects of low temperature
on bitumen properties are typically evidenced by the glass transition temperature (Tg ). When
temperature is lower than Tg , bitumens are glassy, hard and brittle, whereas for the temperature
higher than Tg visco-elastic properties are exhibited. The transition continues down to the glass
transition which can be seen at the lowest temperature ( − 21.65°C) for Bit-R2. Consequently,
Bit-R2, which includes average value of wax percentage, with the lowest value of Tg may have
more resistance to low-temperature cracking compared to other sources of bitumens at a specific
low temperature.
3.2. Conventional test results

The conventional properties of bitumen samples are presented in Table 3. The effects of wax on
different sources bitumen can be explored using Table 3.
Results indicated that Bit-TR1 with the lowest wax content sample depicted a significant
decrease in penetration value and increase in softening point temperature as compared to
bitumens including relatively high wax content.
The softening point temperature can be used along with the penetration to determine the tem-
perature susceptibility of bitumen. The PI is an indicator of temperature susceptibility of bitumen.
A high PI indicates low temperature susceptibility (Whiteoak & Read, 2003). The results show
that Bit-R1 has the highest PI value and thus depicts lesser temperature susceptibility as com-
pared to other different sources of bitumens. It can be also concluded from the results that limited
air blown bitumen significantly lowers the temperature susceptibility of the samples.
As presented in Table 3, ductility and frass breaking point tests may indicate that Bit-TU
containing the highest content of wax exhibits decreased low-temperature properties due to its
low elasticity (Feng, Yu, & Wu, 2012).
As can be seen in viscosity results at 165°C, there is an acceptable correlation with a regression
coefficient (R2 ) of 0.74 between the wax content obtained by EN 12606-1 and viscosity test
results. Bitumen containing low wax content may also give high viscosity. Bit-TU exhibits low
viscosity value at 165°C due to its containing high wax content. However; there is no relationship
between wax content and viscosity values at 60°C and 135°C. This can be explained by high
melting temperature ranges of waxes.
The most intense bitumen ageing processes take place when bitumen is mixed with hot aggre-
gate in the batching plant’s mixer. Under these circumstances the evaporation of light fractions
and bitumen oxidation are the fastest and most intense, and bitumen rapidly hardens. The pro-
cess is referred to as short-term aging. The hardening of the bitumen is gauged by the ductility,
viscosity at 60°C, retained penetration and softening point temperature difference after RTFOT.
Bit-R2, which includes average value of wax percentage, exhibited a better performance in terms
of retained penetration. However, Bit-I exhibits almost identical values in terms of increase in
softening points after RTFOT compared to other bitumen samples. The highest value in terms of
ductility after RTFOT (120 cm) could be seen in Bit-TR2 containing relatively high wax content
Table 3. Conventional test results of bitumens.

Bitumen Bit-TR1 Bit-TR2 Bit-I Bit-TU Bit-R1 Bit-R2 Bit-R3
Sources Turkey Turkey Iraq Turkmenistan Russia Russia Russia
Penetration grade 50/70 40/60 70/100 50/70 60/90 60/90 70/100
Penetration at 25°C (0.1 mm) 50 48 75 50 68 63 76
Softening point (°C) 54 49.7 48.4 52.6 53.2 52.1 48.4
Penetration Index (PI) − 0.25 − 1.37 − 0.62 − 0.58 0.35 − 0.13 − 0.59
Ductility at 25°C (cm) 64 150 48 35 70 76 109
Fraass breaking (°C) − 12 − 12 − 13 − 11 − 17 − 16 − 18
Viscosity (Pa.s) at 60°C 576.6 258.3 285 236.7 205.6 180.8 189
at 135°C 0.613 0.463 0.400 0.338 0.525 0.488 0.388
at 165°C 0.150 0.125 0.138 0.113 0.150 0.138 0.138
Rolling Thin Film Oven Retained penetration after 62 58 59 41 65 68 55
Road Materials and Pavement Design

Test (RTFOT) (163°C; RTFOT (%)
85 min.)
Softening point diff. after 8.8 4.7 17.4 2.8 7.4 4.9 5
RTFOT (°C)
Ductility at 25°C after 14 120 14 8 35 33 58
RTFOT (cm)
Viscosity at 60°C after 1291.7 575.3 1193.3 555.8 478.8 630.0 636
RTFOT (Pa.s)
Hardening factor (the ratio 2.2 2.2 4.2 2.3 2.3 3.5 3.4
of the dynamic viscosity
after RTFOT to dynamic
viscosity before aging at
60°C)
1277
as compared to other short-term-aged bitumens. Thus, low-temperature failure resistance can

be improved by Bit-TR2 before and after the aging process. In this study, the hardening factor
was calculated as the ratio of the dynamic viscosity after RTFOT to dynamic viscosity before
aging at 60°C for different sources of bitumens. A desirable bitumen would have a comparatively
low value of hardening factor which indicates that the viscosity of the bitumen increases slowly
with oxidation. As presented in Table 3, the value of the hardening factor depends on the source
of bitumens. Bit-TU and all Russia bitumen samples (Bit-R1, Bit-R2 and Bit-R3) have lower
hardening factor than Bit-I, and Turkey bitumen samples (Bit-TR1 and Bit-TR2) have the lowest
hardening factor. Bit-I hardens and oxidises much faster than other different sources of bitumens.
On the other hand, the utilisation of Bit-TR1 and Bit-TR2 is expected to provide a positive effect
on pavement performance over time.
3.3. BBR test results

The BBR test was conducted to identify the impact of different contents of wax on the bitu-
men samples under low temperatures. The BBR test was performed at temperatures of − 6°C,
− 12°C, − 18°C and − 24°C for aged (RTFOT and PAV) bitumen samples. The creep stiffness
(S) and slope of the stiffness curve (m-value) are determined from BBR tests and presented in
Table 4. The increment in stiffness values indicates that thermal stresses develop in the pavement
and thermal cracking becomes more likely due to low temperature. On the other hand, reduction
in m-value indicates probability of thermal cracking. Superpave specification requires a maxi-
mum limitation of 300 MPa for stiffness and minimum 0.300 for m-value (ASTM D6648-01,
2001).
As can be seen in Table 4, for all low temperatures, the highest increase in creep stiffness
values was observed in Bit-TR2 and Bit-TU containing the highest amount of wax. This implies
that the bitumen becomes harder with the increment in wax content.
As presented in Table 4, at all test temperatures, creep stiffness parameters of all bitumen
samples depicted values lower than 300 MPa. Since the creep stiffness values were lower than
300 MPa, the low-temperature PG value has been determined on the basis of m-value higher
than 0.3.
As can be seen, as temperature decreases, the m-value exhibits values higher than the specifi-
cation limit. It can be concluded from Table 4 that the PG lower critical temperature of Bit-TR1
containing the lowest wax content ( − 28°C) is lower than other bitumen samples. There is
no significant variation for lower critical temperature values of Bit-TR1, Bit-I, Bit-R1, Bit-R2
and Bit-R3 ( − 22°C). Besides, Bit-TU including the highest wax content has the highest PG
lower critical temperature ( − 16°C). A correlation exists (R2 = 0.78) between the wax content
Table 4. Creep stiffness and m-value of bitumen samples at a loading time 60 s and after different
temperatures.
Creep stiffness (MPa) m-value

Bitumens − 6°C − 12°C − 18°C − 24°C − 6°C − 12°C − 18°C − 24°C
Bit-TR1 – 88.57 170.08 246.00 – 0.338 0.309 0.295
Bit-TR2 – 258.19 519.96 764.69 – 0.311 0.219 0.162
Bit-I – 65.12 95.93 135.53 – 0.334 0.261 0.241
Bit-TU 43.28 101.08 175.97 – 0.317 0.297 0.236 –
Bit-R1 – 60.32 117.37 167.17 – 0.330 0.273 0.257
Bit-R2 – 71.79 146.60 209.84 – 0.307 0.271 0.249
Bit-R3 – 74.03 136.85 219.69 – 0.370 0.289 0.260
obtained by EN 12606-1 and PG lower critical temperature of bitumen. This indicates that high
wax content decreases the resistance of bitumen to low-temperature cracking.
3.4. Rheological test results

This section includes the results of rheological tests applied on all of the bitumen samples
obtained from the different sources. The results have been presented into three groups of DSR
test results, ZSV test results and MSCR test results.
3.4.1. DSR test results

The determination of complex rheological properties of bitumen is currently possible with the
utilisation of DSR. Parameters most commonly tested in DSR include the bitumen complex shear
modulus (G*) and phase angle (δ), tested in various temperature and frequency ranges.
In order to determine upper critical temperature used in the PG system, unaged and RTFOT-
aged specimens of bitumens containing different contents of wax were subjected to oscillating
shear in the DSR at a frequency of 10 rad/s (1.59 Hz). The temperature cycles were set to start at
52°C for unaged and 64°C for RTFOT-aged samples and run up in 6°C increments. The upper
critical temperatures (Tcrit ) used in the PG system were determined for each sample using the
obtained G*/sin δ results and DSR specifications for the PG bitumen. In the PG system, the
upper critical temperature is the temperature at which G*/sin δ = 1.0 kPa for unaged bitumen,
and G*/sin δ = 2.2 kPa for RTFOT-aged bitumen (Asphalt Institute, 2003). The upper critical
temperatures (Tcrit ) for all samples are presented in Table 5.
It can be concluded from the DSR test results that there is an acceptable correlation with a
regression coefficient (R2 ) of 0.78 between the wax content obtained by EN 12606-1 and PG
upper critical temperatures. As can be seen in Table 5, PG upper critical temperature of Bit-TR1
(Tcrit ) containing the lowest wax content is higher than other bitumen samples. On the other
hand, Bit-TU containing the highest wax content has the lowest PG upper critical temperature.
There is no significant variation for Tcrit values of Bit-TR2, Bit-I, Bit-R1, Bit-R2 and Bit-R3.
A higher Tcrit value is an indicator of higher resistance to permanent deformation. Specification
limits of G*/sin δ values for unaged Bit-I sample and RTFOT-aged Bit-I sample do not fix at
the same temperature. The lower temperature (64°C) was selected to be in the safe range as PG
upper critical temperature. Difference of G*/sin δ values for unaged and RTFOT-aged sample
implies that Bit-I hardens and oxidises much faster than other bitumen samples because of the
aging process.
All of the RTFOT-aged samples including different contents of wax were subjected to oscil-
lating shear in the DSR at low (0.01 Hz) and high (10 Hz) frequency levels at five different
temperature cycles ranging from 40°C to 80°C with 10°C increment. The variation of G*/sin δ
(rutting parameter) values of the samples at low and high frequencies are presented in Figures 3
and 4, respectively.
As presented in Figures 3 and 4, in all bitumen samples, G*/sin δ values increase with decrease
in temperature at both frequencies. An increment in G*/sin δ value indicates higher performance
against rutting. Besides, as expected, G*/sin δ values increase with an increase in frequency for
all the bitumen samples. This is due to the rheological behaviour of the bitumen since bitumens
under shorter loading times (high frequency level) exhibit elastic behaviour (Whiteoak & Read,
2003).
As can be seen in Figures 3 and 4, the Bit-TU sample containing the highest wax content
depicted the lowest G*/sin δ value at both high and low frequencies and at all temperatures.
Among the bitumen samples which contain low wax content, the highest value in the G*/sin δ
Table 5. Determination of PG upper critical temperatures for different sources of bitumens.
DSR, G*/sin δ (Pa)

Bitumen Sources Temperature (°C) Non-aged Aged Performance grades
Bit-TR1 Turkey 52 1.25E + 04 PG 70-28

58 5918
64 2820 5816
70 1384 2868
76 702 1462
Bit-TR2 Turkey 52 8047 PG 64-22
58 3493
64 1592 3356
70 779 1493
Bit-I Iraq 52 5160 PG 64-22
58 2253
64 1012 117E + 04
70 460.9 5837
76 2791
82 1307
Bit-TU Turkmenistan 52 3888 PG 58-16
58 1783 3654
64 818 1693
Bit-R1 Russia 52 7006 PG 64-22
58 3392
64 1628 4009
70 797.5 1903
58 3241
64 1551 3650
70 769.7 1775
58 2431
64 1147 3346
70 556.7 1648
values can be seen in the Bit-TR1 sample at 10 Hz frequency and all temperatures. However, this
case is only valid for Bit-TR1 at a low frequency level (0.01 Hz) and at 40°C, 50°C and 60°C.
Under longer loading times (at a low frequency level), a significant increase in G*/sin δ values
can be seen in the Bit-I sample at intermediate temperature levels (40°C, 50°C and 60°C). Among
the Russia bitumen samples, the limited air blown Bit-R1 sample contains the lowest amount of
wax and a significant increase in G*/sin δ values can be seen at Bit-R1 at all frequencies and
temperatures. The effects of Bit-R1 on G*/sin δ values are more obvious at lower frequencies at
all temperature levels.
Fatigue properties of bitumen can be evaluated by the fatigue factor at intermediate tempera-
tures. The fatigue behaviour was investigated by applying continuous oscillatory shear loadings
using DSR. The temperature sweep test is performed under the strain controlled mode at a
frequency of 10 rad/s (1.59 Hz). The temperature cycles were set to start at 40°C within the
PAV-aged samples and run up in 3°C decrements. During the test procedure, an 8-mm diameter
plate with a 2 mm gap between parallel plates was used for each PAV-aged bitumen sample.
There is a limiting maximum stiffness at the intermediate temperature to mitigate fatigue crack-
ing. G*.sin δ values of PAV-aged bitumen samples do not exceed 5000 kPa and low values of
these parameters are considered good indicators of fatigue cracking resistance (Asphalt Institute,
Figure 3. G*/sin δ values for different sources of bitumens at 0.01 Hz.
Figure 4. G*/sin δ values for different sources of bitumens at 10 Hz.
2003). There was a variation in the fatigue parameters (G*.sin δ) for PAV-aged bitumens con-
taining different contents of wax at different intermediate temperatures and these temperatures
were plotted against the wax content according to EN 12606-1 and are illustrated in Figures 5
and 6, respectively.
Figure 5. G*.sin δ values for different sources of bitumens.
Figure 6. Correlation between the wax content by EN 12606-1 and the temperatures at critical G*.sin δ
values of each bitumen under long-term aging.
As depicted in Figure 5, in all bitumen samples, G*.sin δ values increase with decrease in
temperature at 10 rad/s. Owing to the aging, the lower G*.sin δ value indicates the less shearing
energy loss and the better ability for fatigue resistance (Ali, Mashaan, & Karim, 2013). Bit-TR1
and Bit-I samples containing the lowest wax contents depict the highest G*.sin δ value at all
intermediate temperatures. On the other hand, Figure 5 confirms the superior fatigue performance
of Bit-R3 and Bit-TU at all intermediate temperatures with the lowest value of G*.sin δ. Higher
G*.sin δ values are not preferable since the samples with higher G*.sin δ values exhibit fatigue
cracking.
The specification limit values (5000 kPa) are reached with Bit-TR1, Bit-TR2, Bit-I samples,
which occur at test temperature of 25°C, 19°C and 22°C, respectively. In Bit-R1 and Bit-R2 they
occur at the test temperature of 16°C as well as Bit-R3 and Bit-TU meet the specification limit
at the temperature of 13°C. It can be seen that Bit-TR2 has improved (lowered) the interme-
diate temperature compared to Bit-TR1 and Bit-I, containing the lowest amount of wax. In the
best case, Bit-R3 and Bit-TU caused a drop of 12°C compared to Bit-TR1 including the lowest
amount of wax in intermediate temperatures. Low amount of wax increases G*.sin δ values at
all intermediate temperatures.
Figure 6 exhibits an acceptable correlation with a regression coefficient (R2 ) of 0.604 between
the wax content by EN 12606-1 and the temperatures at critical G*.sin δ values of each bitumen
under long-term aging. In general, the high wax content led to lower temperatures at which
G*.sin δ values are acceptable for the bitumen samples. The increase in wax content has an
obvious effect on long-term-aged bitumen fatigue parameter.
3.4.2. ZSV test results

The ZSV results of all of the bitumen samples including different contents of wax, determined
by the utilisation of the DSR machine applied in creep mode are illustrated in Figure 7.
As depicted in Figure 7, Bit-I and Bit-TR1 samples containing low amount of wax exhibit
higher ZSV value than other bitumen samples. A meaningful correlation exists (R2 = 0.65)
between the wax content obtained by EN 12606-1 and ZSV values. This indicates that the ZSV
values decrease with augmentation in the content of wax in the bitumen samples. A higher ZSV
value indicates higher resistance to permanent deformation under long-term loading (Gungor &
Saglik, 2012). In spite of the fact that Bit-I contains relatively higher wax content than Bit-TR1,
Figure 7. ZSV values for bitumens containing different contents of wax.

there is a slight augmentation in terms of ZSV value of Bit-I compared to Bit-TR1. As can be
seen in Figure 7, no significant variation is seen with Russian bitumens in terms of ZSV values.
A significant decrease in ZSV value can be seen at Bit-TU, which contains the highest content
of wax.
3.4.3. MSCR test results

The percent recovery (R), the non-recoverable compliance (J nr ) at two different stress level of
100 and 3200 Pa and stress sensitivity as well as the percent differences in non-recoverable
compliances (J nr−diff ) of the bitumens are presented in Table 6.
Bit-TU and Bit-TR2 samples containing the highest content of wax have the lowest recovery
at any of the stress levels which indicates that Bit-TU and Bit-TR2 perform with less rutting
resistance than other samples. This can be due to the low stiffness and the low elastic behaviour
of Bit-TU and Bit-TR2 samples. While Bit-I exhibits more recovery at 100 Pa stress levels,
Bit-TR1 has the highest recovery value at 3200 Pa. Higher percent recoveries indicate that the
bitumen can recover a higher portion of its total strain at the end of each loading–unloading
cycle, which is favourable to the resistance of the material to rutting.
Between the wax content obtained by EN 12606-1 and the compliance (J nr ) values, there is a
reasonably good correlation with a regression coefficient (R2 ) of 0.98 and 0.95 in stress levels at
100 and 3200 Pa, respectively. Bit-TR1 with the lowest content of wax has the lowest J nr value.
Lower J nr indicates lower susceptibility of the bituminous material to rutting. Results show that
Bit-TU has the highest the compliance (J nr ) value at 100 and 3200 Pa. It can be concluded that
Bit-TU is the most susceptible sample to rutting. The compliance (J nr ) at two different stress
levels of 100 and 3200 Pa values decrease with decrease in the content of wax in the bitumen
samples.
The stress sensitivity of the bitumens was evaluated by means of the percent differences in
non-recoverable compliances (J nr−diff ). This parameter indicates the percentage of increase in
the J nr value of the bitumen when the stress level is increased from 0.1 to 3.2 kPa. It evaluates
the susceptibility of the bitumens to rutting when unexpected heavy traffic loadings are applied
on the pavement structure or unusually high temperatures are observed in the field.
The percent differences in non-recoverable compliances (J nr−diff ) and stress sensitivity results
at the creep and recovery test are also shown in Table 6. This percent difference is a measure
of the sensitivity of the bitumen to the increase in the stress level; therefore, lower values are
associated with a less stress-sensitive material. The value of the J nr−diff parameter and stress
sensitivity are particularly high for Bit-TU. Therefore, Bit-TU can be considered to be highly
stress sensitive with a creep stress of 3200 Pa.
Table 6. Average values of the MSCR test parameters at 60°C calculated from the test data.
J nr @100 Pa J nr @3200 Stress
Bitumen R @100 Pa (%) R @3200 Pa (%) (1/kPa) Pa (1/kPa) J nr−diff. (%) sensitivity
Bit-TR1 35.029 29.862 0.211 0.231 9.522 0.095

Bit-TR2 5.148 2.688 1.305 1.404 7.596 0.076
Bit-I 43.155 28.095 0.229 0.289 26.555 0.266
Bit-TU 14.738 2.454 2.519 3.729 48.057 0.481
Bit-R1 24.774 10.080 0.826 1.069 29.401 0.294
Bit-R2 23.339 9.509 0.849 1.094 28.649 0.286
Bit-R3 17.455 5.991 1.164 1.474 26.615 0.266
4. Conclusion and recommendations

Based on the results presented in this paper, the following conclusions can be drawn. The EN
12606-1 method gives much lower values in the wax content as compared to DSC. Although both
the DSC and EN 12606-1 methods are basically very different methods, they show a reasonably
good correlation based on the selected bitumen samples in terms of wax content.
Crystallisation starting temperatures (Tic ), wax melted out temperatures (Tfm ) and glass tran-
sition temperatures (Tg ) for waxes are different for different sources of bitumens. It is obvious
that the crystallisation takes place during a range of temperatures, indicating the presence of
molecules with different crystallisation points.
Conventional bitumen tests indicated that limited air blown bitumen significantly lowers tem-
perature susceptibility of samples. Based on the findings from the Brookfield viscosity test, it can
be concluded that the presence of wax decreases viscosity values at 165°C. However, there is no
relationship between wax content and viscosity values at 60°C and 135°C. This can be explained
by high melting temperature ranges of waxes.
The low-temperature properties of bitumens are evaluated through PG lower critical temper-
ature obtained using the BBR test correlates with the increment in wax content. It is found that
Tg results are not related to bitumen wax content. However, the PG lower critical temperature
obtained using the BBR test correlates with the increment in wax content. While the DSC tests
are performed on unaged bitumen samples, bitumen samples are subjected to short-term and
long-term aging procedure in the BBR test. In terms of low-temperature properties of bitumens,
the differences between the test results can be varied with aging procedures.
In the light of the findings, the DSR test results show that wax content had an influence on the
bitumen rheology on rutting and fatigue cracking. A detailed investigation performed using the
DSR test indicates that bitumen containing the highest wax content depicts lower G*/sin δ value
than other bitumen samples, thereby possibly decreasing the rutting resistance at high tempera-
tures. Under the PAV aging condition, the temperature of bitumens of high wax content is lower
than that for bitumen with low wax content at the time the stiffness value of G*.sin δ reaches 5000
kPa. It indicates that high wax content positively affects the intermediate temperature stability of
bitumens under the long-term aging condition.
In the light of the findings from ZSV values, it is concluded that the utilisation of bitumen
containing low amount of wax improves rutting performance of mixtures. This can be due to
high viscosity and low wax content, which give the mixture stability at service temperature.
According to MSCR test results, bitumen containing the lowest content of wax has the high-
est recovery and the lowest J nr values in any of the stress levels. Higher percent recovery and
lower non-recoverable compliances may suggest that bitumens are less prone to rutting after the
application of loading–unloading cycles at a common high temperature. In terms of the asphalt
mixture, bitumens with lower J nr values and/or higher recovery values will contribute less to the
accumulation of unrecovered strain in the asphalt layer.
In terms of this study, conventional and rheological bitumen tests have been conducted to
evaluate the rheological properties of waxy bitumens obtained from different sources. It is rec-
ommended to perform rheological tests on different sources of bitumen involving different types
of polymers in order to reduce negative effects of waxes.
Acknowledgements
The authors are thankful to the ABZ-1 Group for their support for performing laboratory tests.
Disclosure statement
No potential conflict of interest was reported by the authors.
ORCiD
Burak Sengoz http://orcid.org/0000-0003-0684-4880
References
Ali, A. H., Mashaan, N. S., & Karim, M. R. (2013). Investigations of physical and rheological prop-
erties of aged rubberised bitumen. Advances in Materials Science and Engineering, 2013, 1–8.
doi:10.1155/2013/239036
Asphalt Institute. (2003). Performance graded asphalt binder specification and testing (Manual Series No.
1, (SP-1)). Lexington: Asphalt Institute.
ASTM D113-86. (1994). Standard test method for ductility of bituminous materials. West Conshohocken,
PA: American Society for Testing and Materials.
ASTM D2872-12. (2012). Standard test method for effect of heat and air on a moving film of asphalt
(rolling thin-film oven test). West Conshohocken, PA: American Society for Testing and Materials.
ASTM D36-06. (2006). Test method for softening point of bitumen (ring-and-ball apparatus). West
Conshohocken, PA: American Society for Testing and Materials.
ASTM D4402-06. (2002). Standard test method for viscosity determination of asphalt at elevated tem-
peratures using a rotational viscometer. West Conshohocken, PA: American Society for Testing and
Materials.
ASTM D4419-90. (2015). Standard test method for measurement of transition temperatures of petroleum
waxes by differential scanning calorimetry (DSC). West Conshohocken, PA: American Society for
Testing and Materials.
ASTM D5-06. (2006). Standard test method for penetration of bituminous materials. West Conshohocken,
PA: American Society for Testing and Materials.
ASTM D6521-05. (2005). Standard practice for accelerated aging of asphalt binder using a pressurized
aging vessel (PAV). West Conshohocken, PA: American Society for Testing and Materials.
ASTM D6648-01. (2001). Standard test method for determining the flexural creep stiffness of asphalt binder
using the bending beam rheometer (BBR). West Conshohocken, PA: American Society for Testing and
Materials.
ASTM D7405-08. (2008). Standard test method for multiple stress creep and recovery (MSCR) of asphalt
binder using a dynamic shear rheometer. West Conshohocken, PA: American Society for Testing and
Materials.
Baldino, N., Gabriele, D., Rossi, C. O., Seta, L., Lupi, F. R., & Caputo, P. (2012). Low temperature rheol-
ogy of polyphosphoric acid (PPA) added bitumen. Construction and Building Materials, 36, 592–596.
doi:10.1016/j.conbuildmat.2012.06.011
Canestrari, F., Graziani, A.Pannunzio, V., & Bahia, H. U. (2013). Rheological properties of bitumi-
nous binders with synthetic wax. International Journal of Pavement Research and Technology, 6(1),
15–21.
CEN TS 15325. (2008). Bitumen and bituminous binders: Determination of zero shear viscosity (ZSV)
using a shear stress rheometer in creep mode. Brussels: European Committee for Standardization.
Das, P. K., Kringos, N., Wallqvist, V., & Birgisson, B. (2013). Micromechanical investigation of phase
separation in bitumen by combining AFM with DSC results. Road Materials and Pavement Design,
14, 25–37. doi:10.1080/14680629.2013.774744
De Visscher, J., Soenen, H., Vanelstraete, A., & Redelius, P. A. (2004). Comparison of the zero shear
viscosity from oscillation tests and the repeated creep test. Proceedings of Euroasphalt & Eurobitume
Congress, Vienna, Austria.
Dubois, E., Mehta, D., & Nolan, A. (2014). Correlation between multiple stress creep recovery (MSCR)
results and polymer modification of binder. Construction and Building Materials, 65, 184–190.
doi:10.1016/j.conbuildmat.2014.04.111
Edwards, Y. (2009). Influence of waxes on bitumen and asphalt concrete mixture performance. Road
Materials and Pavement Design, 10(2), 313–335. doi:10.1080/14680629.2009.9690197
Edwards, Y., & Redelius, P. (2003). Rheological effects of waxes in bitumen. Energy and Fuels, 17(3),
511–520. doi:10.1021/ef020202b
Edwards, Y., Tasdemir, Y., & Isacsson, U. (2006). Effects of commercial waxes on asphalt concrete mixtures
performance at low and medium temperatures. Cold Regions Science and Technology, 45(1), 31–41.
doi:10.1016/j.coldregions.2006.01.002
European Standard EN 12593. (2007). Bitumen and bituminous binders – determination of the Fraass
breaking point. Brussels: European Committee for Standardization.
European Standard EN 12606-1. (2007). Bitumen and bituminous binders – determination of the paraffin
wax content – part 1: method by distillation. Brussels: European Committee for Standardization.
Feng, Z., Yu, J., & Wu, S. (2012). Rheological evaluation of bitumen containing different ultraviolet
absorbers. Construction and Building Materials, 29, 591–596. doi:10.1016/j.conbuildmat.2011.11.007
Gungor, A. G., & Saglik, A. (2012). Evaluation of rutting performance of neat and modified binders using
zero shear viscosity. 5th Eurasphalt & Eurobitume Congress, Istanbul, Turkey.
Laukkanen, O., Pellinen, T., & Makowska, M. (2013). Exploring the observed rheological behaviour of
in-situ aged and fresh bitumen employing the colloidal model proposed for bitumen. Proceedings of
the International RILEM Symposium, Stockholm, Sweden.
Lu, X., Kalman, B., & Redelius, P. (2008). A new test method for determination of wax content in crude
oils, residues and bitumens. Fuel, 87(8), 1543–1551. doi:10.1016/j.fuel.2007.08.019
Lu, X., Langton, M., Olofsson, P., & Redelius, P. (2005). Wax morphology in bitumen. Journal of Materials
Science, 40(8), 1893–1900. doi:10.1007/s10853-005-1208-4
Lu, X., & Redelius, P. (2006). Compositional and structural characterization of waxes isolated from
bitumens. Energy & Fuels, 20(2), 653–660. doi:10.1021/ef0503414
Lu, X., & Redelius, P. (2007). Effect of bitumen wax on asphalt mixture performance. Construction and
Building Materials, 21(11), 1961–1970. doi:10.1016/j.conbuildmat.2006.05.048
Lyne, A., Wallqvist, V., & Birgisson, B. (2013). Adhesive surface characteristics of bitumen binders
investigated by atomic force microscopy. Fuel, 113, 248–256. doi:10.1016/j.fuel.2013.05.042
Musser, B. J., & Kilpatrick, P. K. (1998). Molecular characterization of wax isolated from a variety of crude
oils. Energy & Fuels, 12(4), 715–725.
Petersen, J. C., Robertson, R. E., Branthaver, J. F., Harnsberger, P. M., Duvall, J. J., Kim, S. S., . . . Bahia,
H. U. (1994). Binder characterization and evaluation (Report no. SHRP-A-367). Washington, DC:
Strategic Highway Research Programme.
Redelius, P., Lu, X., & Isacsson, U. (2002). Non-classical wax in bitumen. Road Materials and Pavement
Design, 3(1), 7–21. doi:10.1080/14680629.2002.9689913
Redelius, P., & Soenen, H. (2015). Relation between bitumen chemistry and performance. Fuel, 140, 34–43.
doi:10.1016/j.fuel.2014.09.044
Ruan, Y., Davison, R. R., & Glover, C. J. (2003). Oxidation and viscosity hardening of polymer-modified
asphalts. Energy & Fuels, 17(4), 991–998. doi:10.1021/ef020221l
Soenen, H., Besamusca, J., Fischer, H. R., Poulikakos, L. D., Planche, J., Das, P. K., . . . Chailleux, E.
(2013). Laboratory investigation of bitumen based on round robin DSC and AFM tests. Materials and
Structures, 47(7), 1205–1220. doi:10.1617/s11527-013-0123-4
Whiteoak, D., & Read, J. M. (2003). The shell bitumen handbook. London: Thomas Telford Services.
Wong, W., & Li, G. (2009). Analysis of the effect of wax content on bitumen under performance grade
classification. Construction and Building Materials, 23(7), 2504–2510. doi:10.1016/j.conbuildmat.
2009.02.030

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Investigation of rheological effects of waxes on

Julide Oner & Burak Sengoz

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Investigation of rheological eﬀects of waxes on diﬀerent bitumen sources

(Received 5 February 2016; accepted 28 June 2016 )

*Corresponding author. Email: julide.oner@usak.edu.tr

© 2016 Informa UK Limited, trading as Taylor & Francis Group

Table 1. The general description of samples.

Source of bitumens Abbreviation Sample no. Penetration grades

Turkey Bit-TR Bit-TR1 50/70

2.2. Test methods

2.2.2. Diﬀerential scanning calorimetry (DSC)

Figure 1. A typical DSC diagram through the cooling–heating cycles.

2.2.3. Conventional bitumen tests

2.2.4. BBR test

2.2.5. Rheological test methods

ZSV = t/J = 900/(Jf − J15 ) [Pa.s], (1)

3. Results and discussions

Table 2. DSC and EN 12606-1 analysis of bitumens.

Bitumen Bit-TR1 Bit-TR2 Bit-I Bit-TU Bit-R1 Bit-R2 Bit-R3

Sources Turkey Turkey Iraq Turkmenistan Russia Russia Russia

Figure 2. Correlation between the EN 12606-1 and DSC methods.

3.2. Conventional test results

Table 3. Conventional test results of bitumens.

Road Materials and Pavement Design

as compared to other short-term-aged bitumens. Thus, low-temperature failure resistance can

3.3. BBR test results

Creep stiﬀness (MPa) m-value

3.4. Rheological test results

3.4.1. DSR test results

Table 5. Determination of PG upper critical temperatures for diﬀerent sources of bitumens.

DSR, G*/sin δ (Pa)

Bit-TR1 Turkey 52 1.25E + 04 PG 70-28

Figure 3. G*/sin δ values for diﬀerent sources of bitumens at 0.01 Hz.

Figure 4. G*/sin δ values for diﬀerent sources of bitumens at 10 Hz.

Figure 5. G*.sin δ values for diﬀerent sources of bitumens.

3.4.2. ZSV test results

Figure 7. ZSV values for bitumens containing diﬀerent contents of wax.

3.4.3. MSCR test results

Bit-TR1 35.029 29.862 0.211 0.231 9.522 0.095

4. Conclusion and recommendations

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