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Article history: The degradation of asphalt pavement performance is severely affected by the aging of asphalt. In order to
Received 26 November 2018 improve the anti-aging performance of asphalt, it is necessary to study the aging mechanism of asphalt
Received in revised form 4 March 2019 first. The objective of this paper was to systematically study the characteristics and mechanism of short-
Accepted 24 April 2019
term aging of neat asphalt based on rheological indexes and chemical indexes, including complex mod-
Available online 3 May 2019
ulus (G*), phase angle (d), stiffness (S), m-value, fatigue performance parameter (Nf), carbonyl index (IC@O)
and polydispersity (PDI). The short-term aging of asphalt was performed by the rolling thin film oven test
Keywords:
(RTFOT) at different temperatures and durations, the rheological properties were evaluated by the
Asphalt
Short-term aging
dynamic shear rheometer (DSR) and bending beam rheometer (BBR), the chemical indexes were got by
Time-temperature equivalent effect the Fourier transform infrared (FT-IR) and the gel permeation chromatography (GPC). Meanwhile, the
Rheological properties time-temperature equivalent effects based on the high/low-temperature performance of asphalt were
Chemical properties analyzed. The relationships between asphalt rheological properties and chemical indexes were discussed.
Correlation analysis The results showed that the fatigue resistance was most sensitive to aging while compared with the high/
low-temperature performance of asphalt. The indexes including G*, S, and Nf tended to increase as the
aging degree increased, whereas other rheological indexes had opposite trends. According to the chang-
ing characteristics of the high/low-temperature performance of asphalt, a time-temperature equivalent
effect model of asphalt aging was constructed. Moreover, both the oxidation and volatilization of asphalt
components were accelerated as the aging temperature increased, but the volatilization was more sen-
sitive to temperature than the oxidation. Based on the correlation analysis, both IC@O and PDI exhibited
⇑ Corresponding author.
E-mail address: jiangwei@chd.edu.cn (W. Jiang).
https://doi.org/10.1016/j.conbuildmat.2019.04.197
0950-0618/Ó 2019 Elsevier Ltd. All rights reserved.
824 W. Ye et al. / Construction and Building Materials 215 (2019) 823–838
a strong correlation to rheological properties. Therefore, prediction models based on IC@O and PDI were
constructed to predict the rheological properties of aged asphalt.
Ó 2019 Elsevier Ltd. All rights reserved.
by RTFOT, the rheological test equipment such as DSR and BBR, and pated in the aging, 3 of which were used to calculate the mass
the chemical equipment such as FT-IR and GPC. Moreover, the change, and the rest were used for subsequent tests, as shown in
time-temperature equivalent effects in the short-term aging pro- Fig. 2. For the mass change test, the average of the three replicate
cess and the relationships between asphalt rheological properties tests was taken as the final result.
and chemical compositions could be discussed further. What
should be noted is that this study not only lays the foundation 2.2.2. Dynamic shear rheometer (DSR) test
for the anti-aging researches of asphalt in the future but also pro- The discovery hybrid rheometer HR-1 produced by TA instru-
vides useful guidance for the operation of the asphalt industry. ments from America was used to study the rheological properties
of aged and unaged bitumen. The number of replicate samples
used in the DSR test was one. However, repeated tests were per-
2. Materials and methodology
formed on several samples, and the deviations of repeated tests
were small since the excellent accuracy of the DSR. Therefore, in
2.1. Materials
this paper, no repeated samples were tested in the amplitude
sweep, the temperature sweep, and the linear amplitude sweep.
Bitumen A-70, which was bought from Shanxi great road indus-
trial Co., Ltd and produced by S-OIL corporation from South Korea,
2.2.2.1. Amplitude sweep. The amplitude sweep was performed to
was used in this study. The basic performance of the A-70 is pre-
determine the linear viscoelastic (LEV) deformation limit of the
sented in Tables 1. The 70 means that the penetration of that bitu-
bitumen, and the result was shown in Fig. 3. Subsequent DSR tests
men is between 60 and 80.
will be designed based on the LEV deformation limit.
expected strain (%). sulphoxide) should be used to evaluate the aging degree
[34,52,53]. Existing researches had shown that carbonyl had better
2.2.3. Bending beam rheometer (BBR) test stability under high temperature than sulphoxide [96] and usually,
According to ASTM D2872 and ASTM D6648 [93,94], the change of sulphoxide was too small to be perceived in the
the BBR test, which usually conducted at low temperatures short-term aging [97]. Thus, the carbonyl index would be used to
(6 °C, 12 °C, 18 °C and 24 °C), is used to evaluate the determine the aging degree in this study. Besides, it has been
W. Ye et al. / Construction and Building Materials 215 (2019) 823–838 827
Response (mV)
recorded spectra ranges was from 650 cm1 to 4000 cm1 with
4 cm1 resolutions. The number of scanning was 32 times, and 40
the attenuated total reflectance (ATR) with crystal ZnSe was used
for the spectrum collection. Thermo Scientific OMNIC was adopted 30
as spectrum analysis software. Since the ATR can be automatically
locked after reaching the load threshold and bitumen has plasticity 20
at the room temperature, the ATR could extend different bitumen MMS
to a similar thickness when reaching the load threshold, which 10
provides a necessary precondition for the quantitative analysis LMS SMS
method of FT-IR [9]. For the quantitative analysis method, the area 0
between a baseline and the peak line could be measured, which is 14 15 16 17 18 19 20 21
shown in Fig. 4, and then the peak area ratios could be calculated. Elution time (min)
However, there is no uniform standard for quantitative analysis
Fig. 5. An example of the gel permeation spectrogram of bitumen.
by FT-IR on the aging degree of bitumen and different methods
were proposed by previous studies [9,62,75,100–103]. The most
common one was to use the ratio of the peak area at 1700 cm1 represented were the number of molecules that belongs to each
to the sum of the peak areas in the range of 2000 cm1 to size. Then the ratios of each size could be calculated. The number
650 cm1, which is shown by Eq. (5). The number of replicate sam- of replicate samples used in the GPC test was one. However,
ples used in the FT-IR test was three, and the average of three repli- repeated tests were performed on several samples. The deviations
cate tests was used as the final result. of repeated tests were small since the excellent accuracy of the
A1700 GPC. Therefore, in this paper, no repeated samples were tested in
IC¼O ¼ ð5Þ the GPC test.
A1700 þ A1600 þ A1450 þ A1375 þ A870 þ A815 þ A730
In order to study the characteristics of molecular weight distri-
where A1700 means the peak area of the spectral band at 1700 cm1, bution during the short-term aging [107], PDI could be calculated
A1600 means the peak area of the spectral band at 1600 cm1, and so based on Eqs. (6)–(9) [108]:
on. Pn
i¼1 wi M i
Mw ¼ Pn ð6Þ
i¼1 wi
2.2.5. Gel permeation chromatography (GPC) analysis
PL-GPC 50 Integrated GPC/SEC System from Agilent Technolo- Ni Mi
gies was used in this study and tetrahydrofuran (THF) was selected wi ¼ Pn ð7Þ
i¼1 N i M i
as mobile phase solvents in this study. The chromatogram of
molecular weight distribution could be obtained after 30 min. Pn
i¼1 N i M i
The curve was divided into 13 equal parts according to some pre- Mn ¼ Pn ð8Þ
i¼1 N i
vious studies [85,104–106], as shown in Fig. 5. It is defined that the
part 1 5 belong to the large molecular size (LMS), part 6 9
Mw
belong to the middle molecular size (MMS), and the rest belong PDI ¼ ð9Þ
Mn
to the small molecular size (SMS). What the areas under the curve
where Mn is the number average molecular weight and Mw is the
weight average molecular weight; Mi is the molecular mass, wi is
the weight fraction of each type of molecule, and Ni is the number
0.15 of molecules of Mi.
Above the indexes, Mn shows the statistical average molecular
weight of all the molecular in the sample. Compared to Mn, large
molecular weight components are taken into account in Mw, and
O3
the larger molecular weight the component, the more it con-
0.10 tributes to Mw. PDI is used to evaluate the molecular weight distri-
Absorbance
bution broadness of a sample, and the larger the PDI, the broader
the molecular weight [108].
Absorbance
peak area 3. Results and discussion
0.05
3.1. Effect of aging on bitumen performance
2.2
85
2.0
1.8 80
1.6
75
log(G*) (kPa)
1.4
(°)
1.2 70
1.0
65
0.8
0.6 60
0.4
55
50 100 150 200 250 300 350 400 50 100 150 200 250 300 350 400
(a) log(G*) (b )
G* (kPa) (°)
84
190 106 190
93 81
185 185
80 78
°C
°C
67 180 75
180
54 71
175 175
41 68
170 28 170 65
15 62
165 165
3 58
100 150 200 250 300 350 100 150 200 250 300 350
Duration (min) Duration (min)
*
(c) Contour map of log(G ) (d) Contour map of
Fig. 6. High-temperature performance under different aging configurations.
duration, as shown in Fig. 6(a). Besides, as the aging temperature study [73]. However, two different trends of stiffness are found
increases, the slope of log(G*) increases gradually. This is because while in different aging configurations. While under 163 °C and
the aging is accelerated by the increase of temperature. However, 170 °C, as the aging duration increases, stiffness first increases
the phase angle has an opposite tendency with complex modulus, rapidly, and then the rate of growth gradually slows down. But
as shown in Fig. 6(b). As the aging duration increases, the d while under 177 °C, 184 °C and 191 °C, the rate of growth does
decreases, and there is also a strong linear relationship between not slow down. As for m-value, while under 163 °C and 170 °C,
d and aging duration. As the aging temperature increases, the slope as the aging duration increases, m-value first decreases rapidly,
of d decreases gradually. Besides, it could be seen from Fig. 6(c) and and then the rate of decrease gradually slows down. But while
(d) that the complex modulus and phase angle changes slowly first under 177 °C, 184 °C and 191 °C, the rate of decrease does not slow
and then is accelerated, which means that the initial stage of short- down, as shown in Fig. 7(b). This may because only parts of the
term aging has a fewer effect on the high-temperature perfor- light components could be volatilized at 163 °C or 170 °C. Though
mance than the final stage. the light components decrease as aging last, further aging duration
does not cause further volatilization when that parts of compo-
3.1.2. Low-temperature performance nents are completely volatilized. As the temperature increase,
The low-temperature performance of bitumen is evaluated by more and more components could be volatilized, and a higher tem-
the creep stiffness (S) and m-value after 60 s’ loading of BBR. perature would lead to a higher volatilization speed.
According to Fig. 7(a), aging has a negative effect on low- It seems that the low-temperature performance under different
temperature performance, which also has been found in a previous aging configurations has similar results with the high-temperature
W. Ye et al. / Construction and Building Materials 215 (2019) 823–838 829
0.45 300
0.40 250
% (5)
S (MPa)
m
0.35 200
0.30 150
0.25 100
-50 0 50 100 150 200 250 300 350 400 -50 0 50 100 150 200 250 300 350 400
Duration (min) Duration (min)
(a) S (b) m-value
S (MPa) m
297 190 0.401
190
280 0.384
185 185
263 0.367
°C
°C
228 0.332
175 175
211 0.315
176 0.280
165 165
159 0.263
100 150 200 250 300 350 100 150 200 250 300 350
Duration (min) Duration (min)
performance, but it should be noticed that the influence of the ini- bitumen becomes more and more viscous, resulting in an increase
tial stage of short-term aging on the low-temperature performance in fatigue resistance. Besides, it could be seen from Fig. 8(c) and (d)
is more significant than on the high-temperature performance, as that there should be a time-temperature equivalent effect in the
shown in Fig. 7(c) and (d). Thus, it could be inferred that the fatigue resistance of bitumen during the short-term aging, which
low-temperature performance is more sensitive to aging than the is similar to the high-temperature performance and the low-
high-temperature performance. temperature performance of bitumen. According to the change
ratio of rheological properties in the initial stage of aging, as shown
in Figs. 6(c) and (d), 7(c) and (d), and 8(c) and (d), the fatigue resis-
3.1.3. Fatigue resistance tance is most sensitive to aging, followed by the low-temperature
The fatigue resistance of bitumen is evaluated by Nf under dif- performance, and the high-temperature performance is least sensi-
ferent maximum expected strains (cmax = 2.5%, cmax = 5%). Fig. 8 tive to aging.
presents the Nf under different maximum expected strains and
aging configurations. The Nf (cmax = 2.5%) is larger than Nf
(cmax = 5%), but they seemed had a similar tendency. At each aging 3.2. Time-temperature equivalent effect
temperature, as the duration increase, the Nf increases rapidly at
the beginning but is followed by a slower increase. As the temper- According to the rheological properties change characteristics
ature increases, the slope of Nf increases gradually, which means under different aging conditions, it can be inferred that there
the aging is accelerated by the increase of temperature. This may would be a time-temperature equivalent relationship in the
because as the temperature increases, more and more components short-term aging of bitumen base on the high/low-temperature
could be volatilized, and a higher temperature lead to a higher performance. Thus, the sigmoidal function is introduced to investi-
volatilization speed. As the bitumen component volatilizes, the gate the performance conversion under different combinations of
830 W. Ye et al. / Construction and Building Materials 215 (2019) 823–838
0.2
high-temperature performance
low-temperature performance
0.1
0.0
(T)
-0.1
-0.2
-0.3
Fig. 12. FT-IR spectra after aging at 191 and different duration.
bitumen. Since the carbonyl index calculated by the method men- distribution of the carbonyl index in different aging configurations
tioned above is small and is not suitable for comparison directly. is similar to the rheological properties of bitumen, as shown in
Therefore, the index is standardized to [0, 1] and dived into 10 Fig. 13(b). Thus, it could be inferred that there would be correla-
levels, such as [0, 0.1], [0.1, 0.2] and so on, as shown in Fig. 13. tions between the carbonyl index and the rheological properties
Fig. 13(a) presents the carbonyl index under different aging of bitumen.
configurations. While under 163 °C and 170 °C, the carbonyl index Fig. 14 presents the relationship between the carbonyl index
has similar characteristics. As duration increase, the carbonyl index and the high-temperature performance. As the carbonyl index
first increases slowly, and then the growth is accelerated while increases, the complex modulus increases, the phase angle
after aging for 265 min. The slope of the carbonyl index at decreases, the fatigue factor and rutting factor increases, which
177 °C, 184 °C, and 191 °C is greater than the slope of the carbonyl means the high-temperature performance of bitumen has been
index at 163 °C and 170 °C. The reason is that the components in improved. Besides, there is a strong correlation between the car-
bitumen are more active in a high-temperature environment, mak- bonyl index and the high-temperature performance of bitumen.
ing components easier to react with oxygen. At 163 °C and 170 °C, It can be inferred that the increase of high-temperature perfor-
the volatilization of the light components (Aromatics and Satu- mance is mainly caused by the oxidation of bitumen components.
rates) [73] in the bitumen would carry away parts of energy in Thus, it is reasonable to predict the high-temperature performance
the surface of the film, which hinders the oxidation. Besides, the of bitumen by carbonyl index.
W. Ye et al. / Construction and Building Materials 215 (2019) 823–838 833
Fig. 14. The relationship between the carbonyl index and high-temperature performance.
0.40
250
S (MPa)
S
m
m
0.35
200
0.30
150
S=134.7254+152.2984Ic=o
0.25
R2=0.93658
100
0.0 0.2 0.4 0.6 0.8 1.0
IC=O
Fig. 15. The relationship between the carbonyl index and low-temperature
performance. Fig. 16. The relationship between the carbonyl index and fatigue resistance.
Fig. 15 presents the relationship between the carbonyl index 3.3.3. GPC analysis of different aging configurations
and the low-temperature performance. As the carbonyl index As mentioned in 2.2.5, the peak area of the molecular weight
increases, the stiffness of bitumen increases and the m-value distribution indicates the number of molecules in the region, and
decreases. Besides, there is a strong correlation between the car- the more the number of molecules, the larger the peak area.
bonyl index and the low-temperature performance of bitumen, Fig. 17(a) presents the molecular weight distribution of the bitu-
and the correlation coefficient between the stiffness and the car- men sample aged under 177 °C. It could be seen from the figure
bonyl index is better than the correlation coefficient between the that the components migrations caused by aging mainly occur in
m-value and the carbonyl index. It can be inferred that the MMS and LMS. Fig. 17(b)(f) presents the molecular weight distri-
decrease of low-temperature performance is mainly caused by butions of bitumen under different aging configurations. At each
the oxidation of bitumen components, but the ability to relax from aging temperature, as the duration increases, the SMS and MMS
stress is also affected by other factors. However, it seems still fea- decreases gradually, but the LMS increases gradually. It is because
sible to predict the low-temperature performance of bitumen by the components of bitumen during aging are converting toward
the carbonyl index. the adjacent larger molecular size components, which means the
Fig. 16 presents the relationship between the carbonyl index SMS is converted to the MMS and LMS, and the MMS is converted
and fatigue resistance. It could be seen from the fitting results that to the LMS. For components like saturates, aromatics, resins, and
there is a good correlation between the carbonyl index and fatigue asphaltenes (SARA), the convert could be considered as that from
resistance, which suggests the increase of fatigue resistance may aromatics to resins, and from resins to asphaltenes [109]. However,
be caused by the oxidation of bitumen components. Thus, it seems it should be noticed that when after experiencing a specific aging
feasible to predict the fatigue resistance of bitumen by the car- duration, the SMS starts to increase rather than decrease, as shown
bonyl index. in Fig. 17(b)(f). The reason may because while the SMS and MMS
834 W. Ye et al. / Construction and Building Materials 215 (2019) 823–838
70 @177
100
0 min 13% 12% SMS
16% 15% 13% 13% 14%
60 85 min MMS
145 min 80 LMS
Response (mV)
50 205 min
265 min
Content (%)
325 min 60
40 64% 64%
65% 64% 62%
385 min 67% 65%
30 40
20
20
100 100
14% 13% 12% 12% 13% SMS 15% 14% 11% 12% SMS
16% 15% 16% 15% 15%
MMS MMS
80 LMS 80 LMS
Content (%)
Content (%)
60 60
63% 62% 61% 62% 61%
65% 64% 63% 63% 63%
67% 66% 67% 65%
40 40
20 20
(c)170 (d)177
100 100
14% 14% 12% 13% SMS 13% 12% 13% 10% 11% 10% SMS
16% 15% 15% 16%
MMS MMS
80 LMS 80 LMS
Content (%)
Content (%)
60
59% 60 61% 59% 59%
61% 59% 58% 63% 61% 60%
63% 62%
67% 67%
40 40
20 20
27% 29% 29% 27% 27% 29% 29% 31%
22% 23% 25% 24%
17% 17%
0 0
0 85 145 205 265 325 385 0 85 145 205 265 325 385
Duration@184 (min) Duration@191 (min)
(e)184 (f)191
Fig. 17. The transformation process of molecular size caused by aging.
are still converting to LMS, the LMS is decomposing into the SMS has strong correlations with the rheological properties of bitumen
after absorbing too many smaller molecules. The results are consistent with the conclusions obtained above. On
Fig. 18 represents the relationships between the polydispersity the one hand, a part of saturates and aromatics is converted to
and the rheological properties. The PDI, calculated by Mw and Mn, resins and asphaltenes by oxidation and composition. On the other
W. Ye et al. / Construction and Building Materials 215 (2019) 823–838 835
5.0 (1) As the aging situation shift from 163 °C/85 min to
191 °C/385 min, the G* at 64 °C, S at 12 °C and the Nf
4.5 (cmax = 2.5%) and Nf (cmax = 5%) increase, the d at 64 °C and
m-value decrease. Besides, according to the slopes of indexes
PDI
Table 2
Formulas for predicting rheological properties.
Predicting formulas R2
2 3 0.96909
G ¼ 22:065 þ 22:091IC¼O þ 52:006PDI 25:584PDI þ 3:5455PDI
d ¼ 30:778 12:100IC¼O þ 88:360PDI 21:102PDI2 þ 1:5236PDI3 0.96128
S ¼ 34:709 þ 83:352IC¼O þ 93:784PDI 16:761PDI2 þ 1:4531PDI3 0.97536
m ¼ 0:93567 0:049342IC¼O 0:31204PDI þ 0:055959PDI2 0:0036034PDI3 0.93456
N f ðcmax ¼ 2:5%Þ ¼ 2:1149 107 þ 2:1857 106 IC¼O 1:7712 107 PDI þ 4:7754 106 PDI2 3:9849 105 PDI3 0.93181
N f ðcmax ¼ 5%Þ ¼ 2:2418 105 þ 2:9599 104 IC¼O 1:8975 105 PDI þ 5:6073 104 PDI2 4:9478 103 PDI3 0.96550
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