Construction and Building Materials 76 (2015) 380387

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Construction and Building Materials

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

High temperature performance evaluation of bio-oil modied asphalt

binders using the DSR and MSCR tests
Xu Yang 1, Zhanping You
Department of Civil and Environmental Engineering, Michigan Technological University, Houghton, MI 49931-1295, United States

h i g h l i g h t s
 The high temperature performance of bio-oil modied asphalt were investigated.
 DSR test and MSCR test were utilized to characterize the high temperature performance.
 Three types of waste wood resourced bio-oils were used to modify asphalt.
 The effect of bio-oils on asphalt high temperature performance were evaluated.
 The results from the DSR test and MSCR test were compared.

a r t i c l e

i n f o

Article history:
Received 9 May 2014
Received in revised form 11 October 2014
Accepted 27 November 2014

Keywords:
Bio-oil
Modied asphalt
Rheology
High temperature performance
DSR
MSCR
Statistical analysis

a b s t r a c t
The high temperature performance of bio-oil modied asphalt binders were evaluated using dynamic
shear rheometer (DSR) and multiple stress creep recovery (MSCR) tests. Three types of bio-oils generated
from waste woods were investigated: untreated bio-oil (UTB), treated bio-oil (TB) and polymer modied
bio-oil (PMB). The control asphalt binder (PG58-28) was blended with 5% and 10% bio-oils to prepare
bio-oil modied asphalt binders. Dynamic shear modulus (|G|) and phase angle (d) as well as high temperature stability index (|G|/sin d) were evaluated through the DSR test, while non-recoverable creep
compliance (Jnr) and percent recovery were investigated using the MSCR test. Both the DSR and MSCR test
results showed that the addition of the bio-oils improved the high temperature stability of asphalt binder
with respect to higher |G|, lower d, lower Jnr and higher percent recovery. In detail, with the increase of
bio-oil percentage, asphalt high temperature performance was improved. The statistical analysis showed
that such improvement was statistically signicant. In terms of the comparison among the three types of
bio-oils, it was found that results from the DSR and MSCR tests were slightly different. In the DSR test, the
UTB modied binders showed slightly weaker high temperature stability than the TB and PMB modied
binders, which was mainly due to the high moisture content in the UTB. Whereas in the MSCR test, the
PMB modied binder showed slightly weaker high temperature stability than the UTB and TB modied
binders, which was attributed to the low fraction of polymer (only 0.4% by weight) in the PMB modied
binder. The slight inconsistency between the DSR and MSCR test was likely due to different loading magnitude and loading mode of the two tests. The study also suggests that it is preferable to conduct both the
DSR and MSCR tests to obtain a comprehensive understanding of asphalt high temperature performance.
2014 Elsevier Ltd. All rights reserved.

1. Introduction
1.1. Bio-oil
Bio-oils generated from biomass materials are regarded as
potential alternative binders used in exible pavement. Overall,
Corresponding author at: Department of Civil and Environmental Engineering,
Michigan Technological University, 1400 Townsend Drive, Houghton, MI 499311295, United States. Tel.: +1 906 487 1059 (O); fax: +1 (906)487 1620.
E-mail addresses: xyang2@mtu.edu (X. Yang), zyou@mtu.edu (Z. You).
1
Tel.: +1 9063707996 (O); fax: +1 (906)487 1620.
http://dx.doi.org/10.1016/j.conbuildmat.2014.11.063
0950-0618/ 2014 Elsevier Ltd. All rights reserved.

bio-oils can be generated from a wide range of biomass materials,

such as wood, algae, grass, cornstover, waste cooking oil, and animal waste. Some basic physical and chemical properties of bio-oils
have been investigated in previous studies [14]. Several technologies have been developed to generate bio-oils. Fast pyrolysis has
been proved to be a highly effective approach due to the high yield
rate of bio-oils. Some mature fast pyrolysis equipment has been
developed to produce bio-oils in the United States [4,5]. In fast
pyrolysis, source materials are heated quickly to 400500C with
the absence of air. During this process, the biomass is decomposed
to vapor and chars. The vapor is cooled down quickly to obtain gas

X. Yang, Z. You / Construction and Building Materials 76 (2015) 380387

and liquid. The gas can go back as a heat source while the liquid is
separated as bio-oil. Newly produced bio-oil usually contains some
amount of moisture, which is from the source materials. Previous
studies showed that the moisture content can be reduced by heating bio-oils at a temperature slightly higher than the boiling point
of water [6].
Overall, bio-oil has similar components as petroleum asphalt
binder. The components can be categorized into saturates, aromatics, polars and asphaltenes [7]. However, the elemental composition of bio-oil differs signicantly from petroleum asphalt per the
higher oxygen content in bio-oil [4,8,9]. Some other characteristics
of bio-oil as compared to petroleum asphalt include lower pH and
inhomogeneity [10]. In regard of the effect of bio-oils on asphalt
binder performance, it was found that bio-oils from different
resources can have various functions. Bio-oils derived from animal
waste can improve asphalt low temperature performance
[4,11,12]. Wen et al. [13] found that the bio-oil generated from
waste cooking oils can also improve the low temperature performance of asphalt binder. Asli et al. [14] found that the addition
of waste cooking oil can signicantly reduce the softening point
and viscosity of aged asphalt binder. On the other hand, it was
found that bio-oils generated from wood resources can improve
asphalt high temperature stability while compromise low temperature performance [3,15]. In addition, previous studies suggested
that bio-oils are more susceptible to a high temperature aging as
compared to the petroleum asphalt [11,15].
1.2. Asphalt high temperature performance
Asphalt high temperature performance is related to rutting
resistance of asphalt pavement. Several approaches have been
developed to evaluate the high temperature performance of
asphalt mixture, such as direct rutting resistance testing: asphalt
pavement analyzer (APA) and Hamburg wheel-tracking test. Previous studies also revealed that ow number and dynamic modulus
have a high correlation to rutting resistance of asphalt mixture
[1618]. Some approaches have also been developed to evaluate
the high temperature performance of asphalt binder, such as penetration test, dynamic shear rheometer (DSR) test, and multiple
stress creep recovery (MSCR) test. Penetration test estimates the
high temperature performance based on asphalt stiffness. The
detailed information of the test can be found in ASTM D5 [19]. Penetration test covers the typical service temperature of asphalt
pavement. It is also quick and inexpensive. However, the limitation
of penetration test is also obvious. It is an empirical method without taking account into the fundamental engineering properties of
asphalt. DSR test can overcome this limitation as it measures
asphalt rheological property in a wide range of temperature and
frequency. It is a currently used approach by most agencies in
the United States. DSR test has been used to characterize the high
temperature performance of asphalt binders in many previous
studies [2024]. The detailed information of the test is specied
in ASTM D7175 [25]. Superpave asphalt mixture design recommends the |G|/sin d at 1.59 Hz as the rutting potential index. The
main shortage of the DSR test is that the strain level is low (about
10%), which may underestimate the performance of some modied
asphalt binders because the modiers are not fully activated at a
low strain level [26]. In this regard, the MSCR was developed, as
specied in ASTM D7405 [27]. According to the study by the Federal Highway Administration (FHWA) [26], non-recoverable creep
compliance (Jnr) in MSCR test has a much higher correlation with
asphalt pavement rutting performance as compared to the rutting
index |G|/sin d. Wasange et al. [28] also designed tests to correlate
MSCR results to asphalt mix rutting. In addition, some parameters
that can impact MSCR reliability were explored by Motamed and
Bahia [29], such as geometry, temperature, stress level and loading

381

duration. Recently, MSCR test has been widely used to evaluate

asphalt high temperature performance [30,31].
2. Motivations and research objectives
Although some previous studies reported the effect of bio-oils
on asphalt high temperature performances using DSR, they mainly
focused on the rutting index (|G|/sin d). The detailed effect of biooils on asphalt |G| and d was not well reported in previous studies
[4,11,15]. Moreover, since it was found that the DSR test may be
not capable to well reveal the high temperature performance of
some modied asphalt binders [26], MSCR test was selected to
determine if it can provide more reliable results for bio-oil modied asphalt. The comparison between DSR and MSCR tests on
bio-oil modied asphalt may be a good case study for future
researches to understand how DSR test results differ from MSCR
test results.
The main objective of this study is to evaluate the high temperature performance of bio-oil modied asphalt binders using both
DSR and MSCR test. The effects of bio-oil on asphalt |G|, d, Jnr
and percent recovery will be explored, respectively. Results from
the DSR and MSCR tests were also compared to understand if the
two approaches bring similar ndings. In order to achieve the goal,
three types of bio-oils generated from waste woods were investigated: the untreated bio-oil, treated bio-oil and polymer modied
bio-oil. The petroleum asphalt binder was blended with 5% and
10% bio-oils to prepare bio-oil modied asphalt binders. The
dynamic shear modulus (|G|) and phase angle (d) as well as the
high temperature stability index |G|/sin d were evaluated through
the DSR test, while the Jnr and percent recovery were investigated
using the MSCR test. Statistical analysis was conducted to
understand if the effects are statistically signicant.
3. Materials and preparation
The asphalt binder used in this study was the performance grade asphalt PG5828, meaning the highest and lowest working temperatures are 58 and 28 C,
respectively. PG58-28 is a widely used asphalt in northern region of United States.
The high temperature performance of the PG58-28 in this study has not been
improved by other modiers. The bio-oils used in this study were derived from
waste woods collected in Upper Michigan through a fast pyrolysis. There is a moisture content of 1530% by weight in the newly produced bio-oil, also named
untreated bio-oil (UTB) in this study. A dewatered bio-oil with moisture content
of 58% was obtained by heating the newly produced bio-oil at 110 C, which
was named as the treated bio-oil (TB) in this study. In addition, a polymer modied
bio-oil (PMB) was prepared by adding 4% of polyethylene into the treated bio-oil.
Previous studies showed that polyethylene can improve asphalt high temperature
performance [3235]. Specically, Punith and Veeraragavan [33] stated that a 5%
content of polyethylene is adequate to enhance asphalt binder performance. To produce bio-oil modied asphalt binder, the UTB, TB and PMB were added into the control asphalt by 5% and 10%, respectively. Thus, a total of seven asphalt binders were
investigated in this study: the control asphalt binder, and the 5% UTB, 10% UTB, 5%
TB, 10% TB, 5% PMB and 10% PMB modied asphalt binders. The mixing process was
conducted with a high shear mixer. Some elemental and chemical compositions of
the untreated bio-oil is shown in Table 1.

4. Experimental plan
4.1. DSR test
As previously mentioned, the DSR test was developed to characterize the viscoelastic property of asphalt binders in a wide range of temperature and frequency. In
this study, the DSR test was conducted by a rheometer model Bohlin CVO 120. The
water bath was used to control the temperature. A sinusoidal shear load was
applied on the binder specimen to obtain the dynamic shear modulus (|G|) and
the phase angle (d). The maximum shear strain level was controlled as 10%. The
effect of the bio-oils on the |G| and d was also investigated. The rutting potential
index |G|/sin d at 1.59 Hz was then calculated to evaluate the high temperature performance. The testing temperatures were selected as 58, 64 and 70 C considering
this study aims to investigate the high temperature performance. The testing frequencies were 0.1, 1, 5, 10 and 25 Hz to covers a wide range. All the samples had
been subjected to the standard RTFO test to gain a short term aging before the

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X. Yang, Z. You / Construction and Building Materials 76 (2015) 380387

Table 1
Some compositions of the bio-oil used for this study.
Test values

Carbon (wt%)
Hydrogen (wt%)
Nitrogen (wt%)
Insoluble (wt%)
Solids (wt%)

59.5
6.6
0.37
42.94
2.20

0.22

Shear strain

Properties

0.24

0.2

DSR test. The procedures of the standard RTFO test followed the ASTM D2872 [36].
In the standard RTFO test, the binders were conditioned at 163 C for 85 min with
abundant fresh air. Three replicates were used for each type of binder.

0.18

4.2. MSCR test

The MSCR test was also conducted in the DSR machine. The testing temperature
was 58 C, which is the highest work temperature of the control asphalt binder
PG58-28. A water bath was used to control the temperature. All the binders had
experienced the standard RTFO aging before the MSCR test. Three replicates were
used for each type of binder. The specimen diameter and thickness were 25 and
1 mm, respectively. A one-second shear creep load was applied on the sample, followed by a nine-second recovery. First ten cycles of creep and recovery were conducted under the shear load of 0.1 kPa. Then a 3.2 kPa of shear load was applied on
the same specimen for another 10 cycles. Fig. 1 shows the typical MSCR test results
with 10 cycles of creep and recovery. Because the strain patterns are slightly different from cycle to cycle, an average strain level was calculated to provide a direct
plot for an easier following, as shown in Fig. 2. As previously stated, Jnr is the rutting
potential index in MSCR test, while percent recovery reects the elasticity of
asphalt binder. Thus, both Jnr and percent recovery were investigated to evaluate
the effect of bio-oils on asphalt high temperature performance. The expressions
of Jnr and percent recovery are shown as follows:

Jnr

Nonrecov erable strain

Stress lev el

% recov ery

Recov ered strain

Maximum strain

5. Results and discussion

5.1. The DSR test
Dynamic shear modulus (|G|) and phase angle (d) were
obtained from the DSR test at ve frequencies and four temperatures. A master curve was constructed for each type of asphalt
binder based on timetemperature superposition. The detailed
procedure to construct the master curve can be found in the
authors previous study [15]. The reference temperature to
construct master curve was 58 C.
Fig. 3 shows the |G| master curves of the control binder and the
bio-oil modied asphalt binders. Smooth curves were obtained in

Shear strain

0.24

0.22

0.2

0.18
0

20

40

60

80

Loading me (s)

Fig. 1. Typical MSCR test results with 10 cycles of creep and recovery.

100

10

Creep and recovery Time (s)

Fig. 2. Averaged result from the ten cycles of creep and recovery.

terms of the |G| versus reduced frequency. The |G| increased with
the increase of the reduced frequency. In terms of the bio-oils
effects on asphalt |G|, it was observed that the bio-oil modied
asphalt binder had higher |G| values than the control asphalt binder. The effect of bio-oil on the asphalt |G| was assessed by calculating the |G| increase at each test condition. In this regard, the |G|
values of 5% and 10% UTB modied asphalt binders were 23.4% and
28.0% higher than that of the control binder on average, respectively; the 5% TB, 10% TB, 5% PMB, and 10% PMB modied asphalt
binders had |G| 23.8%, 50.3%, 38.4% and 43.9% higher than the control asphalt binder, respectively. This indicates the addition of the
bio-oils can increase asphalt |G|. In detail, with the increase of the
bio-oil percent, the asphalt binder |G| also increased. The comparison among the three bio-oil modiers showed that the TB and
PMB modied binders owned higher |G| values as compared to
the UTB modied binder. This is mainly due to the higher moisture
content in the UTB as moisture reduced the overall stiffness of
asphalt binder. The PMB and TB modied binders showed overall
close |G| values. Despite that previous studies have revealed that
polyethylene can enhance the high temperature stiffness of asphalt
binder [3335], the PMB did not show visible higher |G|. This was
mainly due to the low polyethylene content in the PMB modied
binder.
The phase angle master curves of the control asphalt binder and
three bio-oil modied binders were plot in Fig. 4. Overall, the phase
angle decreased with the increase of the reduced frequency for the
control asphalt binder. Asphalt binder is a visco-elastic material.
The viscous property is dominant at high temperature whereas
the elastic property is dominant at low temperature. A high
reduced frequency is corresponding to a low temperature and high
frequency. Therefore, the phase angle master curve for the control
asphalt binder was as expected. Further observation showed that
four out of the six bio-oil modied asphalt binders exhibited a
maximum phase angle value when the reduced frequency kept
going up. This phenomenon is similar as that occurs for the phase
angle of asphalt mixture. Previous studies showed that there exists
a maximum phase angle value for asphalt mixture because the
aggregate structure will endure some applied load when the temperature keeps increasing [37]. In this regard, one possible reason
for the phase angle master curve in this study is that there were
some tiny particles or solids that affect the homogeneity of the
asphalt binders. In fact, it was found that bio-oil contains a small
amount of char particles, which can serve as a catalyst and stimulates bio-oil aging when temperature is high [38]. Since the bio-oil
modied asphalt binders had experienced a short-term aging
before the DSR test, there may exist some amount of chars, which
plays similar roles as the aggregate. The gas chromatographymass

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X. Yang, Z. You / Construction and Building Materials 76 (2015) 380387

(a)1.0E+6

(a) 100
Control

10% UTB

10% UTB

5% UTB

Control

5% UTB

95

1.0E+5

90

Phase angle ()

|G*| (Pa)

1.0E+4
1.0E+3
1.0E+2
1.0E+1
1.0E+0
0.01

80
75
70
65

0.1

10

100
60
0.01

Reduced frequency (Hz)

(b) 1.0E+6

85

0.1

10

100

Reduced frequency (Hz)

10% TB

Control

5% TB

(b) 100

1.0E+5

5% TB

Control

10% TB

1.0E+4

90

Phase angle ()

|G*| (Pa)

95

1.0E+3
1.0E+2
1.0E+1
1.0E+0
0.01

80
75
70
65

0.1

10

100
60
0.01

Reduced frequency (Hz)

0.1

10

100

Reduced frequency (Hz)

(c) 1.0E+6
Control

10% PMB

(c) 100

5% PMB

Control

1.0E+5

10% PMB

5% PMB

95

1.0E+4

90

Phase angle ()

|G*| (Pa)

85

1.0E+3
1.0E+2
1.0E+1

85
80
75
70

1.0E+0
0.01

0.1

10

100

65

Reduced frequency (Hz)

Fig. 3. Dynamic shear moduli of control, and UTB and TB modied asphalt binders:
(a) control, 5% UTB and 10% UTB; (b) control, 5% TB and 10% TB; and (c) control, 5%
PMB and 10% PMB.

spectrometry (GCMS) test showed that the bio-oils in this study

contain about 2% solids by weight. This may also contribute to
the phase angle change. In addition, since the thickness of the
samples is only 1 mm, the effect of char particles and solids can
be visibly reected by the phase angle results.
The effect of bio-oils on phase angle can also be obtained from
Fig. 4. Overall, the bio-oil modied binders had lower phase angles
as compared to the control asphalt binder. The phase angle of UTB,
TB and PMB modied asphalt binders were averagely 1.4, 5.4 and
3.0 lower than that of the control asphalt binder, respectively. This
indicates that the addition of bio-oil increased the elastic portion of
the asphalt binder. Comparison among the three types of bio-oils
showed that TB had the most signicant effect on the asphalt
phase angle, followed by the PMB and UTB.
As previously mentioned, |G|/sin d is an index of asphalt high
temperature stability, so a higher |G| and lower d is desirable for

60
0.01

0.1

10

100

Reduced frequency (Hz)

Fig. 4. The phase angles of control, and UTB and TB modied asphalt binders: (a)
control, 5% UTB and 10% UTB; (b) control, 5% TB and 10% TB; and (c) control, 5% PMB
and 10% PMB.

high temperature performance. Above analysis showed that the

three bio-oils in this study can increase |G| while reduce d, so it
is safe to assert that the bio-oils have a positive effect on asphalt
high temperature performance. In detail, the |G|/sin d values of
the control asphalt binder and the bio-oil modied asphalt binders
at 1.59 Hz and 58 C were obtained, as shown in Fig. 5. Overall,
with the increase of the bio-oil concentration, the |G|/sin d also
increased. The |G|/sin d values of 5% UTB, 10% UTB, 5% TB, 10%
TB, 5% PMB, and 10% PMB modied asphalt binders were 23.7%,
29.8%, 28.5%, 55.9%, 42.0%, and 48.3% higher than that of the control asphalt binder, respectively. Comparison among the three
bio-oils showed that the UTB modied asphalt binder had lower

X. Yang, Z. You / Construction and Building Materials 76 (2015) 380387

2.5

15

4000

12

1.5

2000

1000

0.5

3000

control

5% UTB 10% UTB

5% TB

(b)

Jnr (kPa-1)

high temperature stability index than the TB and PMB modied

binders.
5.2. The MSCR test
Figs. 6 and 7 display the MSCR test results of the control asphalt
binder and the bio-oil modied asphalt binders at shear stress level
of 0.1 and 3.2 kPa, respectively. The data results included a onesecond creep phase and a nine-second recovery phase. In the creep
phase, the actual strain level went up with the increase of the loading time. In the recovery section, the strain recovered quickly at the
beginning but the recovery rate decreased with time. The test
results overall were a reection of the visco-elasticplastic property of asphalt binders. After the removal of the creep load, the

(a) 0.30
0.25
0.20
0.15
5% TB

10% TB

5% UTB

10% UTB

5% PMB

10% PMB

0.10
Control

0.05
0.00
0

10

Creep and recovery Time (s)

(b) 12
10
8
6
4
2

5% TB

10% TB

5% PMB

10% PMB

5% UTB

10% UTB

Control

0
0

10

Creep and recovery Time (s)

Fig. 6. The MSCR results of the seven asphalt binders tested at: (a) 0.1 kPa and (b)
3.2 kPa.

Control 5% UTB 10% UTB 5% TB

10% TB 5% PMB 10% PMB

Fig. 5. High temperature stability index |G|/sin d at 58 C and 1.59 Hz.

Actual strain

% Recovery

5000

Actual strain

18
Jnr

% Recovery

(a) 3

Jnr (kPa-1)

|G*|/sin (Pa)

6000

10% TB 5% PMB 10% PMB

8

4
Jnr

% Recovery

3.5

2.5

1.5

0.5

% Recovery

384

0
Control 5% UTB 10% UTB 5% TB

10% TB 5% PMB 10% PMB

Fig. 7. The non-recoverable compliance (Jnr) and % recovery tested at: (a) 0.1 kPa
and (b) 3.2 kPa.

elastic strain was recovered immediately, while some viscous

strain was recovered gradually. It was as expected that the maximum strain level of sample creeping at 3.2 kPa was much higher
than that of samples creeping at 0.1 kPa. It was also as expected
that the strain percent recovery of the sample creeping at 3.2 kPa
was much lower than that of samples creeping at 0.1 kPa. Take
the control binder for instance, the maximum strain level and
the percent recovery loaded at 0.1 kPa were 0.294% and 4.58%,
respectively; while the maximum strain level and the percent
recovery loaded at 3.2 kPa were 10.65% and 1.25%, respectively.
This indicates that with the increase of the creep load level, the
maximum strain level also increases whereas the percent recovery
decreases. The study conducted by FHWA [26] proposed Jnr and
percent recovery as an indexes of high temperature stability and
elasticity. According to this, Fig. 7 displayed the Jnr and percent
recovery of the control asphalt binder and the bio-oil modied
binders. It was observed that a higher creep loading level also
resulted in a higher Jnr. This was mainly due to the higher
permanent deformation and lower percent recovery when the
creep loading level increases.
In terms of the effect of bio-oils on the MSCR test results, it was
observed that all of the bio-oil modied asphalt binders had lower
strain levels and Jnr as compared to the control asphalt binder. For
the creep loading level of 0.1 kPa, the Jnr of 5% UTB, 10% UTB, 5% TB,
10% TB, 5% PMB and 10% PMB were 30.0%, 28.8%, 31.7%, 41.4%,
21.2% and 25.6% lower than that of the control binder, respectively.
For the creep loading level of 3.2 kPa, the Jnr of 5% UTB, 10% UTB, 5%
TB, 10% TB, 5% PMB and 10% PMB were 30.1%, 28.2%, 36.9%, 42.6%,
17.0% and 22.7% lower than that of the control binder, respectively.
Overall, with the increase of the bio-oil content, the Jnr showed a
decreasing trend despite of the close Jnr values between the 5%
and 10% UTB modied binders. The two creep loading levels in
the MSCR test are corresponding to different trafc load levels on
pavement. It is preferable that the positive effect of bio-oil can
be more signicant at higher loading levels. The effect of bio-oils
on the Jnr at the two loading levels suggested that the UTB

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X. Yang, Z. You / Construction and Building Materials 76 (2015) 380387

modication was not sensitive to the loading level change (average

Jnr increase from 29.4% to 29.2%); when the creep loading level
increased, the TB modication effect was slightly enhanced (average Jnr increase from 36.5% to 39.8%), whereas the PMB modication was slightly weakened (average Jnr increase from 23.8% to
19.8%).
It was found that the PMB modied asphalt binders had lower
Jnr than the UTB and TB modied binders. In the DSR test, the
PMB modied binder had slightly higher |G|/sin d than the UTB
modied binders. This indicates that the test results from the
DSR test and the MSCR test were slightly inconsistent. One possible
reason is the different loading types and strain levels between the
DSR and MSCR tests. In the DSR test, the maximum shear strain
level was only 0.1. However, in the MSCR test, the highest shear
strain levels were 0.3 and 10.6 for the 0.1 and 3.2 creep loading levels, respectively. As analyzed above, with the increase of the loading level, the UTB modication did not change visibly; the TB
modication was slightly enhanced; while the PMB modication
was slightly weakened. Although the PMB modication effect is
more signicant than the UTB at a low loading level, it is possible
that the modication effect is lower than the UTB and TB at a high
loading level. This is a possible interpretation for the phenomenon
observed in the DSR and MSCR test. In addition, the polymer is 4%
of the bio-oil and the PMB is 510% of the asphalt in the PMB modied asphalt, so the polymer amount is only 0.20.4% of the
asphalt. This makes the polymer effect on the modication results
very limited. The polystyrene content is normally higher than 3% of
the asphalt binder according to previous studies [33,39]. Other
possible attributions are the different loading modes of the two
tests and the different types of parameters used for the rutting
potential characterization.
In addition to the Jnr, most of the bio-oil modied asphalt binders exhibited a higher percent recovery than the control binder. For
the creep loading level of 0.1 kPa, the percent recovery of 5% UTB,
10% UTB, 5% TB, 10% TB, 5% PMB and 10% PMB were 107.0%, 120.3%,
22.2%, 85.4%, 97.5% and 51.2% higher than that of the control binder, respectively. For the creep loading level of 3.2 kPa, the percent
recovery of 5% UTB, 10% UTB, 5% TB, 10% TB, 5% PMB and 10% PMB
were 58.9%, 7.2%, 78.6%, 95.4%, 114.0% and 47.2% higher than that
of the control binder, respectively. The overall higher percent
recovery indicates that the bio-oils enhanced the asphalt elasticity,
which is also benecial for the permanent deformation resistance.
In terms of the comparison among percent recovery of the three
bio-oils, no signicant differences were observed.

than 0.05. For a specic type of bio-oil, if both the 5% and 10%
bio-oil modied binders have signicant effect on the |G|, then it
is asserted that this type of bio-oil has signicant effect on the
asphalt binder |G|. On the other hand, if neither of them has a signicant effect, it is asserted that this type of bio-oil does not have
signicant effect.
In terms of the |G|/sin d, Jnr and percent recovery, because all of
them were tested at a specic condition, the data variance is much
lower. Therefore, the statistical analysis was conducted using a
general linear model in ANOVA. In the general linear model, the
independent factors were the bio-oil type and the dose level, while
the dependent factor was the |G|/sin d, Jnr and percent recovery. A
95% condence level was also used to determine the effect significance. The ANOVA was carried out in the Minitab 16 statistical
software.
Tables 2 and 3 showed the Wilcoxon signed-rank test results for
the |G| and d through the comparison between the control binder
and the bio-oil modied binders. It was observed that all of the six
p-values were lower than 0.05 in the Wilcoxon signed-rank test for
|G|, indicating that there was a signicant difference. In fact, all of
the p-values were 0. This is because the |G| values of all the bio-oil
modied asphalt were higher than the control asphalt. In other
words, the |G| of the control asphalt binder was signicantly changed after the addition of the bio-oils. In regard of the bio-oil type, it
is safe to assert that all of the three types of bio-oils had signicant
effect on the asphalt binder |G|. In regard of the bio-oil dose level,
it is safe to assert that both the 5% and 10% dose level had signicant effect on the asphalt |G|. It was observed that all of the p-values in the Wilcoxon signed-rank test for the d were lower than 0.05
except for the 5% UTB modied binder. Based on this, it is safe to
assert that both the TB and PMB had signicant effect on the
asphalt phase angle, whereas if the UTB had signicant effect
was still uncertain. Similarly, it is safe to assert that the 10% dose
level had signicant effect on the asphalt phase angle, whereas if
the 5% dose level had signicant effect was still uncertain.
Tables 46 showed the ANOVA results using general linear
model for the |G|/sin d, Jnr and percent recovery, respectively.
The DF represented the degree of freedom. Three types of bio-oils
and three dose levels were analyzed, so the DFs of both bio-oil type
and dose level were 2. If the p-value is lower than 0.05, a signicant
effect would be asserted. From Table 4, it was found that both the
bio-oil dose level and the bio-oil type had signicant effect on the
|G|/sin d. The test results showed that the bio-oil increased |G|/
sin d, indicating the bio-oil content increase can result in a

5.3. Statistical analysis

A statistical analysis was conducted to verify if the bio-oils have
statistically signicant effect on asphalt properties, including |G|,
phase angle, |G|/sin d, Jnr, and percent recovery. Three types of
bio-modiers (the UTB, TB and PMB) and three dose levels (0%,
5%, and 10%) were investigated in this study. In this regard, it is
necessary to understand if the bio-oil type or dose level has significant effects on asphalt properties. A parametric paired t-test was
initially considered for such purpose. However, one assumption
of the paired t-test is that the sample population follows a normal
distribution. Since the |G| and d values were tested in a wide temperature and frequency, the data variance is pretty high. For
instance, the lowest and highest |G| values of the control binder
were about 50 and 50,000 Pa, respectively. Thus, the |G| cannot
be assumed to obey a normal distribution. In this regard, a Wilcoxon signed-rank test was used in this study. The Wilcoxon signedrank test is a non-parametric test that can be an alternative to the
paired t-test when the sample population cannot be assumed to be
normally distributed [40]. A 95% condence level was used, indicating that there is a signicant effect when the p-value is lower

Table 2
The Wilcoxon signed-rank test results for the |G|.
Paired samples

Z-value

P-value

Signicant effect?

Control
Control
Control
Control
Control
Control

4.01
4.01
4.01
4.01
4.01
4.01

0
0
0
0
0
0

Yes
Yes
Yes
Yes
Yes
Yes

and
and
and
and
and
and

5% UTB
10% UTB
5% TB
10% TB
5% PMB
10% PMB

Table 3
The Wilcoxon signed-rank test results for the d.
Paired samples

Z-value

P-value

Signicant effect?

Control
Control
Control
Control
Control
Control

0.99
2.62
4.01
3.28
3.28
3.24

0.32
0.01
0
0.001
0.001
0.001

No
Yes
Yes
Yes
Yes
Yes

and
and
and
and
and
and

5% UTB
10% UTB
5% TB
10% TB
5% PMB
10% PMB

386

X. Yang, Z. You / Construction and Building Materials 76 (2015) 380387

Table 4
ANOVA results using the general linear model for |G|/sin d at 1.59 Hz and 58 C.
Source

DF

Signicant effect?

Bio-oil dose level (0%, 5%, 10%)

Bio-oil type (UTB, TB, and PMB)

2
2

11.85
4.89

0.004
0.041

Yes
Yes

Table 5
ANOVA results using the general linear model for Jnr.
Source

DF

Signicant effect?

Bio-oil dose level (0%, 5%, 10%)

Bio-oil type (UTB, TB, and PMB)

2
2

9.01
4.29

0.007
0.049

Yes
Yes

Table 6
ANOVA results using the general linear model for percent recovery.
Source

DF

Signicant effect?

Bio-oil dose level (0%, 5%, 10%)

Bio-oil type (UTB, TB, and PMB)

2
2

0.34
0.07

0.721
0.937

No
No

statistically signicant increase on the |G|/sin d. It also suggests

that different types of bio-oils had signicantly different effects
on the |G|/sin d. From Table 5, both the dose level and type had signicant effect on the Jnr. Discussion above showed that the addition
of bio-oil reduced the Jnr. Therefore, it indicates that when the
bio-oil content goes up, Jnr is expected to reduce signicantly.
Meanwhile, different types of bio-oils had signicantly different
effect on the Jnr. From Table 6, it was observed that neither the
bio-oil dose level nor the bio-oil type had signicant effect on
the percent recovery. This indicates that the addition of bio-oil
had no signicant effect on the percent recovery of asphalt binder.

6. Findings and conclusions

This study investigated the effect of three types of bio-oils (the
UTB, TB and PMB) generated from waste woods on asphalt high
temperature performance. By adding 5% and 10% bio-oil into the
control asphalt binder, a total of seven asphalt binders were prepared, which are the control asphalt binder, and the 5% UTB, 10%
UTB, 5% TB, 10% TB, 5% PMB, and 10% PMB modied binders. DSR
and MSCR tests that can characterize asphalt high temperature
performance were conducted on the RTFO aged binders to obtain
the dynamic shear modulus (|G|), phase angle, |G|/sin d, nonrecoverable creep compliance (Jnr), and percent recovery. The
effects of the bio-oils on asphalt properties were discussed, and a
statistical analysis was conducted to verify if the effects are
statistically signicant.
From the DSR test, the addition of bio-oil increased asphalt |G|,
reduced the phase angle, and increased the rutting potential index
|G|/sin d, indicating that the bio-oils can improve asphalt high
temperature stability. From the MSCR test, the addition of bio-oil
reduced the non-recoverable creep compliance (Jnr) and increased
the percent recovery, also indicating the improvement of high temperature stability and elasticity. The statistical analysis showed
that the effect of bio-oil on the |G|, d, |G|/sin d, and Jnr are statistically signicant. Thus, it is concluded that the bio-oils used in this
study can improve asphalt high temperature performance.
In terms of the comparison among the three types of bio-oils,
the test results from the DSR test and the MSCR test were slightly
inconsistent. In the DSR test, the effect of UTB on the |G|, phase
angle, and |G|/sin d were lower than that of the TB and PMB. This
is due to the higher moisture content in the UTB. In the MSCR test,
the PMB performed weaker than the UTB and TB. One possible

reason for the inconsistent results was the different loading levels
and loading modes, because the strain level in the DSR test was
much lower than that in the MSCR test. In addition, since the polymer fraction of the PMB modied asphalt was pretty low (0.4% by
weight), it is acceptable that its performance did not surpass other
two types of bio-oils. In addition, it also indicates that the high
temperature performance evaluation from DSR test may vary from
that in MSCR test, so it is preferable to conduct both the tests to
obtain a comprehensive result.
Acknowledgments
The research work was partially sponsored by the Federal Highway Administration through Michigan Department of Transportation (MDOT). The authors also appreciate the guidance and
involvement of Nathan Maack, Andre Clover, Benjamin Krom, and
John Barak of MDOT. This research could not have been completed
without the contributions of Dr. R. Christopher Williams. The
authors appreciate Christopher DeDene, James Vivian, Morgan
Hensen for the assistance on materials and data collection. MDOT
assumes no liability for its content or use thereof. The content of
this paper reects the views of the authors, which is responsible
for the accuracy of the information presented herein. The contents
may not necessarily reect the views of MDOT and do not constitute standards, specications, or regulations.
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