Construction

and Building

Construction and Building Materials 21 (2007) 1961–1970

MATERIALS
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Effect of bitumen wax on asphalt mixture performance

Xiaohu Lu *, Per Redelius
Nynas Bitumen, SE-149 82 Nynashamn, Sweden

Received 2 June 2005; received in revised form 28 January 2006; accepted 31 May 2006
Available online 25 September 2006

Abstract

This paper mainly deals with waxes which are naturally present in bitumens, and does not include synthetic waxes that sometimes are
proposed as bitumen additives. The main objectives were to study the rheological effect of bitumen waxes and the impact of waxy bit-
umens on asphalt mixture performance, such as rutting, low temperature cracking, and water sensitivity. In the rheological character-
isation of bitumens, a dynamic shear rheometer (DSR) and bending beam rheometer (BBR), as well as various conventional
methods, were used. For asphalt mixtures, rutting, low temperature cracking and water sensitivity were evaluated by wheel tracking test
(WTT), thermal stress restrained specimen test (TSRST), and modified Lottman test, respectively. It was found that, at high service tem-
peratures and within the same bitumen grade, differences in rutting between the asphalt mixtures made with waxy and non-waxy bitu-
mens were relatively small. However, the presence of wax in bitumen resulted in physical hardening at low temperatures. Using waxy
bitumens, asphalt mixtures tended to show higher fracture temperature. As regards water sensitivity, no effect of the wax content in bitu-
men was seen. The water sensitivity was however heavily influenced by type of aggregate and to less extent by bitumen type. The present
study implies that the effect of wax on bitumen quality and asphalt mixture performance depends on many factors. Those may include
the chemical composition of the bitumen and particularly the nature of the wax.
 2006 Elsevier Ltd. All rights reserved.

Keywords: Bitumen wax; Asphalt mixture performance; Rutting; Low temperature cracking; Water sensitivity

1. Introduction The presence of waxes in bitumen was usually consid-

Bitumen has been used in road construction and in
many other applications for a long time. The material
can be produced from crude oils or found in nature as nat-
ural asphalt. The composition of bitumen is complicated
and is not completely known. The complexity is primarily
caused by a large variety of chemical compounds that con-
stitute bitumen. In bitumen production through distilla-
tion, the wax which may be present in crude oils can be
retained in the bitumen. The wax may be types of paraffin
wax or microcrystalline wax [1–4]. Paraffin wax refers to
the group of n-alkanes with few or no branches, while
microcrystalline wax mainly consists of naphthens and
iso-paraffins.
*
Corresponding author. Tel.: +46 8 52065007; fax: +46 8 5206 5454.
E-mail address: xiaohu.lu@nynas.com (X. Lu).
ered detrimental [5]. As a consequence, in some countries
like Germany, France, and China, a limit of wax content
was included in binder specifications. This was mostly
based on assumption that the melting of waxes at high tem-
peratures reduced asphalt mixture’s resistance to rutting
and that the crystallisation of wax at low temperatures con-
tributed to mixture cracking. The physical hardening (stiff-
ening due to molecular structuring) and poor binder
adhesion to aggregate were also considered to associate
with wax content.
In literature, the effects of waxes on bitumen quality and
mixture performance were reported different [6–12]. The
debate on waxy bitumen was complicated by the lack of
precise definition of wax, differences in wax type, as well
as poor precision of test methods [7,13]. For one and the
same bitumen, wax content determined by different meth-
ods can differ significantly. For example, the wax in
AAM-1 (a SHRP core asphalt) was reported as about 4%

0950-0618/$ - see front matter  2006 Elsevier Ltd. All rights reserved.
doi:10.1016/j.conbuildmat.2006.05.048
1962 X. Lu, P. Redelius / Construction and Building Materials 21 (2007) 1961–1970

in reference [14], while in reference [6] more than 25% wax
was reported. Another example is that in the European
bitumen specification EN 12591, two methods (distillation
and extraction) were included for determination of wax
content, and maximum values are 2.2% and 4.5%, respec-
tively. The differences suggest that the wax fraction was
not well defined and can be influenced by the test methods
used.
The main objectives of this paper were to study the rhe-
ological effect of bitumen waxes and to determine the
impact of bitumen wax on asphalt mixture performance
characteristics, such as rutting, low temperature cracking,
and water sensitivity. Relationships between the properties
of asphalt mixtures and binders were also investigated. A
wide range of bitumens from different sources were
selected. For determining wax content, differential scan-
ning calorimetry (DSC) and distillation method (EN
12606-1 or DIN 52015) were used. The rheological charac-
terisation of bitumens was performed using a dynamic
shear rheometer (DSR) and bending beam rheometer
(BBR). The asphalt mixtures were evaluated by wheel
tracking test (WTT), tensile stress restrained specimen test
(TSRST), and modified Lottman test.
the slack wax has a lower boiling point and thus molecular
sizes which are smaller or equal to the smallest wax mole-
cules in bitumens.
2.2. Asphalt mixtures
Asphalt mixtures were prepared in accordance with
ABT11 in the Swedish technical directive [15]. This mixture
type is a dense graded asphalt concrete with a maximum
aggregate size of 11 mm, and with about 6.5% (by weight)
binder and 3.5% voids. The particle size distribution of
aggregates is shown in Fig. 1. A laboratory mixer and a
plate compactor with two rubber tyres (diameter 400 mm
and width 80 mm) were employed to produce asphalt mix-
ture slabs, 600 · 400 · 60 mm for WTT, and 600 · 400 ·
100 mm for specimen preparation in TSRST. In these
slabs, crushed granite aggregates (Farsta) were used. For
the testing of water sensitivity, cylindrical specimens
100
90
Passing
80 Min
Passing by Weight (%)

2. Materials Max
70

2.1. Bitumens 60

50
Bitumens of different sources and of different grades (50/
40
70, 70/100, and 160/220 according to the European Stan-
dard EN 12591) were investigated. The results of conven- 30
tional tests are summarised in Table 1. For comparison, 20
a sample (Bitumen G) of 160/220 was also prepared at lab-
10
oratory by adding 6% slack wax to a non-waxy bitumen
(50/70 grade, Venezuela source). The slack wax is a com- 0
0.01 0.1 1 10 100
mercial product with a congealing point of 42.5 C. It is
a mixture of oil and wax and is obtained as a by-product Aggregate Size (mm)
from the dewaxing process of the refining of lubricating Fig. 1. Particle size distribution of aggregate for the Swedish standard
oil. Compared to the waxes naturally present in bitumens, asphalt mixture ABT11.

Table 1
Conventional tests of bitumens
Bitumen Sources Pen at 25 C (0.1 mm) Softening point ( C) Viscosity 135 C (mm2/s) Dynamic viscosity 60 C (Pa s) Fraass
breaking (C)
50/70 grade
A Mixed 65 49.4 481 287 14
70/100 grade
B Venezuela 83 45.4 345 187 21
C Mexico 101 45.1 325 124 16
D Unknown 86 46.4 181 96 16
160/220 grade
E Venezuela 192 37.8 199 64 21
F Venezuela 214 39.1 283 61 22
G Lab blenda 181 39.8 243 70 17
H Russia 180 40.1 202 53 15
I Mid-East 205 39.2 225 53 22
a
Prepared by mixing 6% slack wax with 50/70 non-waxy bitumen (Venezuela source).
 X. Lu, P. Redelius / Construction and Building Materials 21 (2007) 1961–1970
(diameter 100 mm, length 60 mm) were prepared using a
gyratory compactor. The aggregates used were obtained
from two sources, SB (red-grey salic gneiss) and SH (sedi-
ment gneiss).
3. Test methods
3.1. Differential scanning calorimetry (DSC)
DSC procedure has been described previously [5].
Briefly, for each test, about 15 mg bitumen sample was her-
metically sealed into a DSC pan. A matched pan and lid
were used as reference. The sample was heated to 120 C
and held for 15 min. Data were recorded during cooling
to 80 C and heating to 120 C, both at a rate of 10 C/
min. The wax content was calculated from an endothermic
peak during the heating scan (Fig. 2). In the calculation, a
constant melting enthalpy of 121 J/g was used as reference.
By DSC, glass transition temperature, wax crystallisation
starting temperature and melting out temperature were
also determined.
3.2. EN 12606-1 (or DIN 52015)
In this European standard test, a specified distillation
process was used to obtain a waxy distillate from bitumen.
The distillation unit consisted of a distillation flask, a lab-
oratory burner, and Erlenmeyer flask used as distillation
receiver. The waxy distillate was then dissolved in ether/
ethanol (50/50, V/V) solvent and let to crystallise at tem-
peratures down to 20 C. The crystallised waxes were col-
lected by filtration. The test was carried out on two
portions, each with 25 g sample. A detailed description of
the test method can be found in reference [16].
0.3
Cooling at 10˚C/min
0.2
0.1
Heat Flow (w/g)
0 surement device was ±0.02 mm. Rut depth (average) was
-100 -50 0 50 100
-0.1
Base line
-0.2
Heating at 10˚C
endothermic peak
-0.3
Temperature (˚C)
Fig. 2. DSC characterisation of a waxy bitumen D. Wax content is
calculated based on the endothermic peak.
1963
3.3. Rheological tests with a dynamic shear rheometer
(DSR)
The rheological measurements of bitumen were per-
formed at different temperatures (25–70 C) and at different
frequencies (0.005–25 Hz) with a DSR (Rheologia Stress
Tech). In all tests, parallel plates with 25-mm diameter
and 1-mm gap were used. For the preparation of a test
specimen, about 50 g bitumen was heated to 130 C for
1 h, and sufficient sample was poured onto upper plate.
The upper plate with bitumen was set to the rheometer
and the test sample was trimmed with a hot knife at a
gap 1.05 mm. After trimming, the upper plate was lowered
to the testing gap (1 mm). Tests were performed at various
low stresses to ensure the rheological measurements to be
within the linear range. The measured parameters included
complex modulus (G*), complex viscosity (g*) and phase
angle (d).
3.4. Creep tests with bending beam rheometer (BBR)
In the creep test, bitumen beams (125 mm long, 12.5 mm
wide and 6.25 mm thick) were submerged in a constant-
temperature bath and kept at test temperature ( 15,
20, or 25 C) for 1 h. A constant load of 100 g was then
applied to the rectangular beam which was supported at
both ends by stainless steel half-rounds (102 mm apart).
The deflection of center point of the bitumen beam was
measured continuously. Creep stiffness (S) and creep rate
(m) of the bitumen were determined at several loading
times ranging from 8 to 240 s. For the evaluation of phys-
ical hardening, creep response was also measured after
bitumen beam being isothermally stored in the BBR bath
for 24 h.
3.5. Wheel tracking test (WTT)
The tests were performed in a fully automated device
comprising a hydraulic servo system. Asphalt mixture slab
(600 · 400 · 60 mm) was placed in a fixed mould in a con-
trolled climate chamber. The test conditions were as fol-
lows: tyre pressure 0.6 MPa, speed 2.5 km/h, temperature
60 C, and load 5 kN. Data, such as profiles, temperature,
load magnitude, and wheel passes, were acquired by a spe-
cial developed software. The accuracy of laser profile mea-
150 calculated from three cross-profiles (50 mm distance
between two) in the middle of the slab. For each bitumen,
two asphalt mixture slabs were prepared and tested.
3.6. Tensile stress restrained specimen test (TSRST)
In TSRST, cylindrical specimens (diameter 55 mm,
height 250 mm) were horizontally cored from the asphalt
mixture slabs (600 · 400 · 100 mm). The slabs were pre-
pared using a plate compactor, as described in Section
2.2. The asphalt specimen was glued to two aluminium
1964 X. Lu, P. Redelius / Construction and Building Materials 21 (2007) 1961–1970

plates, and then mounted in a load frame. A refrigerating
machine was used to reduce temperature at a rate of
10 C/h. Fracture occurred when thermally induced stress
in the specimen exceeded its strength. The measured
parameters are shown in Fig. 3, which includes fracture
temperature, fracture strength, transition temperature,
transition stress and slope of the elastic part of the stress-
temperature plot.
3.7. Water sensitivity by indirect tensile test
This test is described in the Swedish FAS Method 446
[17]. It is a modified Lottman test and is similar to the
CEN method prEN 12697-12. For each mixture (ABT11
type, 3.5% voids), 10 specimens (diameter 100 mm, length
60 mm) were prepared using a gyratory compactor and
divided into two subsets of five specimens each. A subset
of five specimens was kept at room temperature (or dry
conditions). The other subset of five specimens was vacuum
saturated for 3 h and then conditioned in a water bath at
40 C water for 7 days (i.e. wet conditions). The indirect
tensile tests were performed at 10 C. The indirect tensile
strength ratio (ITSR) was obtained by the average indirect
tensile strength of conditioned specimens divided by that of
control specimens.
6.0
Fracture
strength
ΔT
Thermal Stress (MPa)
4. Results and discussion
4.1. DSC characterisation and determination of bitumen
waxes
The crystallisation or melting of waxes in bitumen
involves energy change. This can be easily determined by
DSC. In Table 2, results of the DSC measurements are
summarised. As indicated, the bitumen samples differ
widely in the wax content (0–6.2%). For the laboratory
blend with slack wax (sample G), the measured value is
lower than the added amount. This could imply certain sol-
ubility of the slack wax in the bitumen and/or impurity of
the wax. It should be noted that the wax content as
calculated by using a constant enthalpy in this study is
not an absolute value. The DSC measures transformation
enthalpy, and in fact different waxes can have different
enthalpies, meaning the calculation of wax content in bitu-
men is relative.
The determination of wax content was also performed
using the European standard method EN 12606-1 (or
DIN 52015). As shown in Table 2, the DIN test gives much
lower values in the wax content as compared with DSC.
Differences between the samples are also reduced consider-
ably in the DIN test. It is believed that the high-tempera-
ture (up to over 500 C) distillation step of the DIN test
may destroy the molecular structure of waxes (thermal
cracking). The resulting smaller paraffin molecules could
be soluble in ether/ethanol and do not crystallise in the sol-
vent at the specified low temperature ( 20 C), leading to
Cooling rate: 10C/h lower apparent wax content. On the other hand, the non-
slope = Δs waxy bitumens (B, E) as defined by DSC may contain mol-
T

Δs ecules with long straight paraffinic side chains. Those

4.0
branches can be split off in the destructive distillation,
which in turn produces certain amount of paraffin wax in
the DIN test. The difference in wax content between the
Fracture temp.

2.0 Stress relaxation two tests might also be due to the wax solubility in the bitu-
men giving no crystallisation/melting response in DSC. A
Transition
temp.

detailed investigation on wax composition and structural

characterisation will be published elsewhere [18].
0.0 The discussion above implies that both DSC and DIN
-45 -35 -25 -15 -5 5
methods are relative in determining wax content in
Temperature (C)
bitumen; but DSC might give more representative values.
Fig. 3. The TSRST test of an asphalt mixture prepared with bitumen E. For clear presentation and convenient discussion in later

Table 2
DSC and DIN analysis of bitumens
Bitumen Wax content Crystallisation starting Melting out Glass transition Wax content by DIN (%)
by DSC (%) temperature by DSC (C) temperature by DSC (C) temperature by DSC (C)
A 2.3 37 84 27 1.0
B 0 – – 17 0.3
C 4.1 46 84 28 1.2
D 6.2 41 74 27 1.7
E 0 – – 20 0.4
F 2.4 31 72 35 1.1
G 2.9 14 63 22 1.4
H 4.1 40 87 28 1.5
I 4.2 39 83 32 1.3
 X. Lu, P. Redelius / Construction and Building Materials 21 (2007) 1961–1970
sections, the wax contents measured by DSC will be mainly
referred to. Although both the DSC method and DIN
method are basically very different with several sources of
uncertainty, they show a reasonably good correlation with
a correlation coefficient (R2) of 0.79. Fig. 4 covers a wider
range of bitumen sources with 17 samples (including the
nine studied in this paper) to have the most reliable
correlation.
4.2. Rutting resistance
4.2.1. Rheological testing of bitumens
Resistance to rutting is one of the most import perfor-
mance requirements for an asphalt mixture. The rutting
performance is mainly determined by type of road con-
struction, aggregate gradation, void content, but also to
some extent by the rheological properties of the bitumen,
such as softening point and dynamic viscosity (Table 1),
and stiffness modulus, etc. It is therefore interesting to
know if/how bitumen rheological parameters are influ-
enced by the wax content. Various rheological parameters
8 statement is based on one single observation on bitumen
Paraffins by DIN 52015 (%)
6
y = 0.352x + 0.31
4 R2 = 0.79
2
0 tion and simplicity can be found in the SHRP report
0 2 4 6
Wax Content by DSC (%)
Fig. 4. Correlation between the DIN and DSC methods. The number of
samples has been extended.
Table 3
Rheological parameters determined by DSR at 60 C
Bitumen G* at 1.59 Hz (kPa) G*/sin d at
1.59 Hz (kPa)
A 2.59 2.61
B 1.77 1.78
C 1.60 1.60
D 0.97 0.98
E 0.57 0.58
F 0.60 0.60
G 0.67 0.67
H 0.55 0.55
I 0.54 0.54
1965
measured using DSR are shown in Table 3. Besides the
SHRP rutting parameter, G*/sin d, it was intended to
include zero shear viscosity (ZSV) in the test program since
ZSV had been shown to be a better rutting indicator [19].
Unfortunately difficulty was observed in precisely defining
ZSV for waxy bitumens in a DSR frequency oscillation
mode, as reported in [20]. Instead, complex viscosity at a
low shear frequency of 0.005 Hz (or low shear viscosity,
LSV), was measured.
The DSR test shows that all the samples at 60 C and
1.59 Hz are essentially viscous (phase angle approaching
90), on which the presence of waxes has no influence. As
a consequence, the SHRP rutting parameter G*/sin d
mainly reflects a contribution of bitumen stiffness or com-
plex modulus; in fact, it is controlled by loss modulus. Also
there is good correlation between G*/sin d and LSV. These
parameters correlate well with conventional dynamic vis-
cosity with correlation coefficients R2 > 0.95. It is found
that all the rheological properties are mainly dependent
on bitumen grade. For the 160/220 grade bitumens, no
effect of wax is observed (see examples of the results in
Fig. 5). For the 70/100 grade, wax may have adverse effect
with respect to binder rutting indicators. However, this
D. It should also be pointed out that bitumen D does not
fully fulfill the binder specification EN 12591 [21] concern-
ing kinematic viscosity at 135C; the viscosity value is
about 20% lower than the criterion. In addition, dynamic
viscosity at 60 C is below the Swedish requirement (mini-
mum 120 Pa s).
4.2.2. Wheel tracking test of asphalt mixtures
In literature, different tests have been used to evaluate
the rutting (permanent deformation) of asphalt mixtures.
Typical types of test included uniaxial stress test, triaxial
stress test, diametral test, and wheel tracking test (WTT).
A comparison of different tests with respect to field simula-
8
3000
G*/sin(delta) at 60˚C and 1.59 Hz (Pa s)
50/70 grade
2500
70/100 grade
160/220 grade
2000
1500
Complex
viscosity at
0.005 Hz (Pa s) 1000
307
204 500
177
115
62 0
0 2 4 6 8
78
70 Wax Content by DSC (%)
65 Fig. 5. Bitumen rheological parameter G*/sin (delta) versus wax content
58 by DSC.
1966 X. Lu, P. Redelius / Construction and Building Materials 21 (2007) 1961–1970

(SHRP-A-415). Of these test methods, WTT (normally at relation coefficients R2 between 0.6 and 0.9. The results
40–50 C) was often recommended for better field simula- indicate that the effect of wax on bitumen rheology and
tion. In this study, WTT was selected and all the tests were mixture rutting is not solely determined by wax content.
performed at 60 C. The use of the relatively high temper- Many factors, particularly bitumen composition and wax
ature was intended to highlight negative effect of the wax characteristics, could play roles [18]. In other words, it
melting on the rutting resistance. This temperature was seems more important to know how wax crystallises/melts
also considered as a typical summer temperature on as temperature changes rather than to get an absolute value
asphalt pavements in the Nordic countries. of wax content.
Fig. 6 shows examples of rutting curves, which are the
average data of two tests (two slabs for each bitumen). 4.3. Low temperature cracking
The rut depths after 1000 and 1500 wheel passes are com-
pared in Fig. 7. As indicated, the asphalt mixtures with 4.3.1. Bitumen tests
harder bitumens (50/70 and 70/100) are more resistant to The low temperature properties of bitumens are evalu-
rutting than those with softer bitumens (160/220). Within ated through different parameters, including Fraass break-
the same bitumen grade, differences between the mixtures ing point (Table 1), glass transition temperature, Tg (Table
are relatively small; the mixtures prepared with waxy bitu- 2), and those obtained using the bending beam rheometer
mens do not show deeper rut as compared to those with (BBR). It is found that Fraass breaking point is not related
non-waxy bitumens. The wheel tracking test of asphalt to bitumen wax content, and relation of Tg to wax content
mixtures correlates with bitumen properties (e.g. softening is very poor (R2 = 0.35). In Fig. 8, bitumen samples are
point, dynamic viscosity, G*, G*/sin d, and LSV) with cor- compared by BBR tests at 15 and 25 C. For each
grade, the samples are arranged in order of the wax con-
tent. Obviously, the bitumens of identical grade may dis-
50 play large differences in the creep response. Differences in

40
1200
1h storage at -15C 24h storage at -15C
Rut Depth (mm)

A B
30 1h storage at -25C 24h storage at -25C
E F 900
Stiffness (MPa)

20
600

10
300

0
0 1000 2000 3000 4000
0
Wheel Passes
A B C D E F G H I
Fig. 6. Result examples of the wheel tracking test at 60 C. Bitumens used a Bitumen Codes
in the asphalt mixtures: A (50/70) and F (160/220) are wax containing
bitumrnd; B (70/100) and E (160/220) are non-waxy. 0.90
1h storage at -15C 24h storage at -15C
1h storage at -25C 24h storage at -25C
50
1000 passes 1500 passes
160/220 grade
45 0.60
70/100 grade
m-value

40
50/70 grade
Rut Depth (mm)

35
30
0.30
25
20
15 50/70 grade 70/100 grade 160/220 grade

10 0.00
5 A B C D E F G H I
0 b Bitumen Codes
A B C D E F G H I
Bitumen ID in Mixture Slabs Fig. 8. Stiffness and m-value measured by BBR at different temperatures
and at a loading time of 60 s. The figure illustrates bitumen dependence of
Fig. 7. Asphalt mixture rutting after 1000 and 1500 wheel passes in WTT. the creep response and effect of isothermal storage.
 X. Lu, P. Redelius / Construction and Building Materials 21 (2007) 1961–1970 1967

stiffness and m-value are not related to the wax content (or For non-waxy bitumens (B, E), values of the hardening
wax crystallisation) of bitumen, again suggesting wax nat- index are close to 1, indicating no physical hardening
ure and bitumen composition can have effects [18]. occurs. For the bitumens containing wax, significant phys-
For further evaluation of wax effect, the limiting temper- ical hardening can be seen. However, statistical correlation
atures (LST – the temperature at 300 MPa stiffness, and between the hardening index and the wax content by DSC
LmT – the temperature at 0.3 m-value) are determined is not strong (R2 < 0.5). The correlation is not improved
from the plots of stiffness and m-value versus temperature. when the bitumens of different grades are examined sepa-
As shown in Table 4, the bitumens differ considerably in rately. At a similar level of wax content, the physical hard-
the limiting temperatures, even within the same grade. ening may differ greatly between the samples. In addition, a
Examples are found for 160/220 bitumens (E, F, G, H, bit better relationship is observed between the hardening
I), where difference in LmT can exceed 10 C. On the other index and the wax content by the DIN method
hand, the bitumens of different grades may have similar (R2 > 0.5). The observations imply that only considering
limiting temperatures (e.g. about 21 C LST for 50/70 wax content is not sufficient to understand its impact. Phys-
A and 160/220 H, and 25 C LmT for 70/100 C and ical hardening is attributed to wax crystallisation, but
160/220 H). However, the limiting temperatures are not could also be due to other mechanisms.
related to the wax content of bitumen, as illustrated in
Table 4
Fig. 9. Some wax-containing bitumens even exhibit lower
Limiting temperatures and physical hardening of bitumens
limiting temperatures than non-waxy bitumens.
Bitumen Limiting temperature Hardening index
As already mentioned, bitumen wax was considered to
contribute to physical hardening at low temperatures. LST (C) LmT (C) At 15 C At 25 C
Physical hardening is a reversible process, which can pro- A 21.3 23.0 1.48 1.14
duce rheological changes without altering the chemical B 18.5 23.3 1.02 1.08
C 22.7 25.5 1.45 1.42
composition of bitumen. In a waxy bitumen, the reversible
D 20.0 21.0 1.45 1.47
process can be the crystallisation/melting of wax. For E 23.0 28.3 1.09 1.04
quantitative evaluation, physical hardening index is F 29.4 34.6 1.37 1.55
defined. It is the ratio of stiffness after 24 h storage to stiff- G 23.6 23.5 1.82 1.22
ness at 1 h storage (cf. Fig. 8). The hardening indices H 21.6 25.0 1.71 1.64
I 23.7 28.0 1.59 1.59
obtained at 15 and 25 C are presented in Table 4.

-15 -15
Limiting Temperature (C)
Limiting Temperatures (C)

70/100 grade LST LST

160/220 grade
LmT LmT

-25 -25

-35 -35
0 2 4 6 8 0 2 4 6
Wax Content by DSC (%) Wax Content by DSC (%)

Fig. 9. The limiting temperatures versus the wax content of bitumen. LST is the temperature at 300 MPa stiffness, while LmT the temperature at m-value
of 0.3.

Table 5
Low temperature properties of asphalt mixtures determined by TSRST
Bitumen in Fracture temperature (C) Fracture strength (MPa) Slope at fracture (MPa/C) Transition temperature (C) Transition
asphalt mixtures stress (MPa)
A 31.4 4.82 0.37 23.7 2.21
B 33.4 4.87 0.32 22.8 1.65
C 33.2 4.54 0.35 25.3 2.00
D 28.4 3.76 0.29 20.9 1.78
E 37.9 4.93 0.33 26.8 1.46
F 41.0 4.68 0.34 32.6 2.06
G 32.3 4.61 0.34 24.0 2.00
H 27.5 3.09 0.24 19.6 1.29
I 31.7 3.34 0.28 24.9 1.54
1968 X. Lu, P. Redelius / Construction and Building Materials 21 (2007) 1961–1970

4.3.2. Tensile stress restrained specimen tests (TSRST) of -20

asphalt mixtures 70/100 grade 160/220 grade

Mixture Fracture Temperature (C)

In determining the low temperature cracking of asphalt
mixtures, TSRST was selected, because this method gave -25
better field prediction according to a previous study [22].
As already shown in Fig. 3, different parameters are deter- -30
mined in TSRST. At the beginning of the test, a relatively
slow increase in the thermal stress is observed, which is due
to relaxation of the specimen. When the temperature is -35
below certain level (transition temperature), the thermally
induced stress is not relaxed and is almost linearly related
to the temperature until fracture of the specimen. At the -40
fracture temperature, the stress reaches the maximum
value, which is referred to as the fracture strength.
-45
In Table 5, average results (two tests for each asphalt 0 2 4 6 8
mixture) are summarised. In general, the TSRST shows Wax Content of Bitumen by DSC (%)
good repeatability. The difference observed in the fracture
temperature between two tests is about 1 C, except for -20
the specimens with bitumen D, for which about 5 C differ- 70/100 grade 160/220 grade

Asphalt Fracture Temperature (C)

ence is observed. The large variation implies that the
-25
asphalt mixture with this bitumen might not be homoge-
nous due to larger and random wax crystals, and thermal
effect on wax crystallisation [23]. -30
The cracking temperature of asphalt mixture does not
simply relate to the wax content of bitumen (Fig. 10).
For the mixtures prepared with relatively hard bitumens -35
(50/70 or 70/100) of 0–4% DSC wax, difference in the frac-
ture temperature is rather small (less than 2 C). In the case -40
of 160/220 bitumens, the fracture temperature may increase
by 5–10 C as the DSC wax exceeding 3% (or the DIN wax
above 1.3%). There is also a significant difference between -45
the bitumens containing similar levels of wax but from dif- 0 0.5 1 1.5 2
ferent sources. For example, at about 4% DSC wax, the Wax Content of Bitumen by DIN Method (%)
mixture prepared with bitumen I shows 4 C lower in the Fig. 10. Asphalt fracture temperature versus wax content in bitumens.
fracture temperature than the mixture with bitumen H.

Table 6
The ITS and ITSR results for the asphalt specimens prepared with different bitumens and aggregates
Bitumen A B C D E F G H I
Aggregate SB ITS (control specimens)
Mean, kPa 2640 2959 2011 2250 1678 1318 1857 2009 1419
CV, % 3.4 2.5 3.1 3.3 3.9 4.3 3.1 2.6 2.4

ITS (conditioned specimens)

Mean, kPa 1794 2157 1541 1887 1174 1021 959 1293 927
CV, % 4.3 7.1 1.5 5.5 2.1 6.8 7.7 1.7 3.0
ITSR, % 68 73 77 84 70 77 52 64 65

Aggregate SH ITS (control specimens)

Mean, kPa 3008 3158 1980 2356 1423 1152 1463 1630 1293
CV, % 4.5 4.0 4.9 2.6 2.6 4.3 4.3 3.1 7.9

ITS (conditioned specimens)

Mean, kPa 2820 2466 1826 1996 1146 911 1115 1183 1065
CV, % 5.0 9.4 6.4 9.5 1.5 13.4 3.4 11.5 4.3
ITSR, % 94 78 92 85 81 79 76 73 82
ITS = indirect tensile strength, ITSR = indirect tensile strength ratio, i.e. ITS (conditioned specimen)/ITS (control specimen), Mean = Mean result of five
tests, CV = coefficient of variation.
 X. Lu, P. Redelius / Construction and Building Materials 21 (2007) 1961–1970 1969

This might be attributed to compositional differences (e.g.
n-paraffins and naphthenes) in the waxes between the bitu-
mens [18]. In addition, bitumen F shows better low temper-
ature performance as compared to the reference non-waxy
bitumen E. However, the slack wax in bitumen sample G
displays an adverse effect on the mixture low temperature
cracking. The laboratory blend was prepared by mixing
6% slack wax to a non-waxy hard bitumen (penetration
55), and the slack wax contained about 50% n-alkanes with
C19 to C36. It is likely that the crystallisation of n-alkanes in
bitumen makes asphalt mixture more susceptible to the low
temperature cracking.
The dependence of asphalt mixture cracking on the low
A or C and with aggregate SH. These mixtures show ITSR
higher than 90%. Interesting cases are also seen for asphalt
mixtures prepared with aggregate SB and with waxy bitu-
mens G (lab blend) and D. The two asphalt mixtures differ
from those with non-waxy bitumens in extremely opposite
80
Aggregate SB
70

ITSR (%)
temperature parameters of bitumen is examined. The best
60
correlation developed is between the mixture fracture tem-
perature and bitumen LmT with a correlation coefficient
R2 of 0.65. The fracture temperature also weakly correlates
with bitumen Fraass breaking point, but not with the glass 50
transition temperature (Tg). It is also found that the transi-
tion temperature of asphalt mixtures and bitumens are not 3.2% 6.0% 3.6% 5.7%
related. This indicates that interactions between fine aggre- voids voids voids voids
40
gates and bitumen molecules make the mechanisms of tran- E G
sition different. Bitumen in Asphalt Mixture

4.4. Water sensitivity 90

Aggregate SH
As described in Section 2.2, the aggregates from two
80
sources, SB (red-grey salic gneiss) and SH (sediment gneiss)
were selected in evaluating the water sensitivity of asphalt
mixtures. The test results according to FAS Method 446 70
ITSR (%)

(cf. Section 3.7) are presented in Table 6. Obviously, there

is an effect from the aggregates. For almost all the bitu-
mens, aggregate SH performs better than SB. Furthermore, 60
the ITSR values are affected by bitumen type, but the
degree of bitumen effect is aggregate dependent. For the
mixtures with aggregate SH, differences in ITSR are smal- 50
ler as compared to those prepared with aggregate SB.
3.2% 5.5% 3.6% 6.1%
Fig. 11 indicates that the ITSR has no relation to the voids voids voids voids
wax content of the bitumens; some asphalt mixtures with 40
E G
waxy bitumens even display higher ITSR (less water sensi-
Bitumen in Asphalt Mixture
tivity) than those with non-waxy bitumens. Examples can
be taken for the asphalt mixtures prepared with bitumen Fig. 12. Effect of void contents on ITSR.

100 100
Aggregate SB
A
C
D
80 80 E D
ITSR (%)

ITSR (%)

B F I
B F C G
E H
A I
60 H 60

G Aggregate SH

40 40
0 2 4 6 8 0 2 4 6 8
Wax Content by DSC (%) Wax Content by DSC (%)

Fig. 11. The ITSR of asphalt mixtures versus bitumen wax content (A–I are bitumen codes).
1970 X. Lu, P. Redelius / Construction and Building Materials 21 (2007) 1961–1970
directions. This is not the case when aggregate SH is
considered.
In addition to ABT11 with 3.5% voids, a few tests were
made for asphalt mixtures of about 6% voids. Two 160/220
bitumens, E (non-wax) and G (lab blend with slack wax),
were used in experiments. As expected, the asphalt mixtures
of higher voids are a more water-sensitive (Fig. 12). But it is
again demonstrated the importance of aggregate in control-
ling the water sensitivity of the mixture specimens.
5. Conclusions
Based on the results presented in this paper, the follow-
ing conclusions can be drawn.
The rheological properties of bitumen at high service
temperatures, in most cases, are not influenced by the
wax content. Within the same bitumen grade, differences
between asphalt mixtures prepared with waxy and non-
waxy bitumens are relatively small. Results of the wheel
tracking test of asphalt mixtures correlate with the rheolog-
ical properties of bitumens.
The low temperature properties of bitumens, such as
stiffness, m-value, limiting temperatures and Fraass break-
ing point, are not simply correlated to the wax content.
However, the presence of wax in bitumen results in physical
hardening. Using waxy bitumens, the asphalt mixtures tend
to have higher fracture temperature. There are significant
differences in the fracture temperature between the samples
with identical wax content but of different bitumen sources.
Relationships between mixture fracture temperature and
bitumen low temperature parameters are generally weak.
The water sensitivity of asphalt mixtures is mainly con-
trolled by the aggregate used. This property may be also
influenced by bitumen type; but the degree of bitumen
effect is aggregate dependent. For the materials tested,
water sensitivity as evaluated by ITSR has no relation to
the wax content of bitumen. Compared to the asphalt mix-
tures prepared from non-waxy bitumens, those with waxy
bitumens show either higher or lower water sensitivity,
depending on bitumen sources.
The study implies that the effect of wax on bitumen
quality and asphalt mixture performance depends on many
factors. Those may include the chemical composition of the
bitumen and particularly the nature of the wax.
Acknowledgements
The authors wish to thank technical staffs at Nynas lab-
oratories, Dr. Safwat Said at the Swedish National Road
and Transport Research Institute, Linköping, for perform-
ing the wheel tracking tests, and Mr. Jones Ekblad at the
Royal Institute of Technology (KTH), Stockholm, for
the TSRST tests.
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