Construction and Building Materials: Meizhu Chen, Feipeng Xiao, Bradley Putman, Bingbing Leng, Shaopeng Wu

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Construction and Building Materials 59 (2014) 10–16

Contents lists available at ScienceDirect

Construction and Building Materials


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

High temperature properties of rejuvenating recovered binder


with rejuvenator, waste cooking and cotton seed oils
Meizhu Chen a, Feipeng Xiao a,⇑, Bradley Putman b, Bingbing Leng a, Shaopeng Wu a
a
State Key Laboratory of Silicate Materials for Architectures, Wuhan Univ. of Technology, Wuhan 430070, China
b
Department of Civil Engineering, Clemson University, USA

h i g h l i g h t s

 Rejuvenator, waste cooking and cotton seed oils were employed for rejuvenation of RAP.
 High temperature characteristics of rejuvenated asphalt binder were tested.
 The used rejuvenated additives can reduce the viscosity value and fail temperature.
 Rejuvenator, cotton seed oil or waste cooking oil result in an increase of phase angle.

a r t i c l e i n f o a b s t r a c t

Article history: Rejuvenator, waste cooking and cotton seed oils contain a great amount of unsaturated fatty acids,
Received 9 January 2014 similar to the light oil component of asphalt binder which usually decreased due to a long term aging
Received in revised form 17 February 2014 procedure. Based on the rejuvenation theory and some related studies, rejuvenator, waste cooking and
Accepted 19 February 2014
cotton seed oils can be used for asphalt regeneration. The objective of this study was to investigate the
Available online 12 March 2014
high temperature rheological properties of rejuvenating aged asphalt binder with rejuvenator, waste
cooking and cotton seed oils. The materials used for this study included three sources of aged asphalt
Keywords:
(recovered from reclaimed asphalt pavement), one virgin asphalt (PG 64-22), and three rejuvenating
Asphalt
Aging
materials: rejuvenator, waste cooking and cotton seed oils with three percentages (0%, 5%, and 10% of
Rejuvenating rejuvenating asphalt). The used mass ratio of aged to virgin asphalt is 1:3 (i.e. 25% aged binder) in this
High temperature properties study. The high temperature characteristics of these rejuvenated asphalts were tested including rutting
Waste cooking oil resistance factor (phase angle and complex modulus), failure temperature and rotational viscosity. The
results indicated that the rutting resistance factor and the complex modulus of rejuvenated binders
decreased due to the addition of rejuvenator, cotton seed oil or waste cooking oil while their phase angles
increased. In addition, the aged asphalt used a small amount of waste cooking oil or cotton seed oil can
more easily achieve the demand of PG 64 binder in rutting resistance factor, phase angle, complex
modulus and failure temperature of aged asphalt compared with rejuvenator. Finally, waste cooking
oil or cotton seed oil can slightly reduce the viscosity value of the aged asphalt and thus decrease the mix-
ing and compaction temperatures of the mixture.
Ó 2014 Elsevier Ltd. All rights reserved.

1. Introduction amount of the reused waste cooking oil accounts for 20–30% of the
total consumption of the cooking oil [1]. The annual waste cooking
Waste cooking oil, a type of the waste greases produced during oil produced in China is about 5–7.5 million tons and only 4 million
the cooking and food processing, contains large amounts of toxic tons can be collected as a recycled resource [1]. Waste cooking oil
substances such as alfatoxin but also is a kind of available resource has become one of the environmental pollutants and seriously
for further recycling. Management of such oils and fats poses a affects the food safety in China. In recent years, the waste cooking
significant challenge because of their disposal problems and possi- oil incidents occur frequently (using wasted cooking oil as a
ble contamination of the water and land resources. In general, the common oil into the food), which seriously endangers the health
of human being.
Some researchers did a lot of research projects in the reuse of
⇑ Corresponding author. Tel.: +1 864 6504821. waste cooking oil [2–4]. One method is to produce soap, which
E-mail address: fpxiao@gmail.com (F. Xiao).

http://dx.doi.org/10.1016/j.conbuildmat.2014.02.032
0950-0618/Ó 2014 Elsevier Ltd. All rights reserved.
M. Chen et al. / Construction and Building Materials 59 (2014) 10–16 11

results in the secondary pollution but the recycled amount of Table 1


waste cooking oil is very limited. Another way is to produce G/sin d and failure temperature values of recovered and virgin asphalt binders.

biodiesel, which has some disadvantages such as high energy con- Testing temperature A B C PG 64-22
sumption and cost. Waste cooking oil, similar to the light oil com- 
G /sin d (kPa) 64 °C 123.31 1.51
ponent in asphalt, contains a lot of unsaturated fatty acids. The oil 70 °C 55.06 0.88
component of asphalt reduces after a long term performance. 76 °C 5.94 24.74 9.64
According to asphalt rejuvenating theory [4–8], a low viscosity 82 °C 2.85 11.30 4.58
88 °C 1.45 5.26 2.29
oil content (i.e. regenerative agent) or softer virgin asphalt can be Failed temp. (°C) 90.8 101.0 91.7 65.8
added into aged asphalt to coordinate its chemical composition
and proportion to produce new asphalt binder. Therefore, waste
cooking oil can be used for asphalt regeneration [9], which may
highest failure temperature while other two aged binders have a similar failure
be expected to increase the utilization of waste cooking oil, with temperature. All rheological tests were performed in accordance with AASHTO
better environmental, social and economic benefits, and capacious and ASTM Superpave specifications in this study.
applications prospects. A US Patent has mentioned that the waste The recovered binder, rejuvenator, and virgin binder (PG 64-22) were blended
cooking oil can be used as a rejuvenator to soften asphalt [10]. at 145 °C and a speed of 200 rpm for 15 min based on their contents. Then samples
were immediately used for viscosity and DSR tests. Viscosity was measured using a
Wen reported that waste cooking oil can be used to produce bioas-
spindle spinning at a 20 rev/min rate according to AASHTO T316 [18] after 30 min
phalt [11]. Asli and Karim [12] used physical index and rheological of thermal stabilization at four different temperatures (e.g. 120, 135,150 and
properties index to evaluate the effect of waste cooking oil on the 160 °C). A number 10 spindle and a specimen weight of 8.5 g were used for this test.
indoor aged asphalt, and concluded that the waste cooking oil can Two replicates were tested for all samples.
be used as a regenerative agent in recycled asphalt which can yield The high temperature rheological properties of each binder were measured
using a DSR at different grade-specific testing temperatures according to AASHTO
the lower penetration value and similar to its original bitumen. T315 [19]. In this research, a one millimeter gap and 25 mm diameter plate for
The cotton seed oil can be edible after refined, but crude cotton all binders were used to obtain DSR values at high temperatures. Each binder was
seed oil can damage sperm cells. The cotton seed oil can also pro- measured in terms of phase angle (d) and complex shear modulus (G) values start-
duce soap and biodiesel, but has the same problem of waste cook- ing from its PG temperature until failed in accordance with Superpave
specifications.
ing oil. The major components of the cotton seed oil is fatty acids,
The grade determination feature of the DSR was used to determine the failure
similar to the light oil component in asphalt, so it can be also used temperature for each sample. This procedure tests the sample at a starting temper-
for asphalt regeneration. ature (i.e., 64 °C for PG 64-22) and increases the temperature to the next PG grade if
To find a more environmentally friendly alternative asphalt is a the G/sin d value is greater than the value required by AASHTO M320 [20]
big challenge. As used in asphalt pavement, bioasphalt should be (1.000 kPa for original binder).

easy to mix and lay down. In addition, it is also stiff enough to


withstand traffic loading. Meanwhile, it should not crack at a rela-
tively low temperature. Asphalt mixture lacking high temperature 3. Results and discussion
stability is prone to yield the permanent deformation at a high per-
formance temperature. State Highway Research Program (SHRP) 3.1. Rutting resistance factor (G/sin d)
indicates that asphalt provides 40% of the rutting resistance ability
of an asphalt mixture [13]. The key to improve the high tempera- G/sin d reflects the irrecoverable deformation of asphalt during
ture resistance to deformation of bituminous pavement is to accu- the loading process. Asphalt, with a higher G/sin d value but a
rately evaluate high temperature performances of asphalt [14–16]. smaller flow deformation at high temperature, has a higher rutting
Consequently, rheology has become a useful tool in characterizing resistance.
the asphalt high temperature performance. SHRP protocol brought Fig. 1 shows that the influence of the amount of R, O or W on the
up a series of tests in a very wide range of temperatures which al- rutting resistance factor of different binders. It was observed that
low obtaining information about the suitability of a given asphalt the rutting resistance factors of the rejuvenated binders strongly
in a further application [17]. depend on the R, O or W contents and the test temperatures.
Some research articles have proven that waste cooking oil is one Generally, their rutting resistance factors decrease as test temper-
of rejuvenating agents that possibly improve the aged bitumen atures and R, O or W concentrations increase. The rejuvenated
properties to the similar level of the virgin bitumen [11,12], but asphalts containing W or O show lower G/sin d values than those
no research was found to compare the effect of waste cooking oil with the same content of R at the same test temperatures. Thus,
to other rejuvenators on rheological properties. Moreover, it is a under the same condition, the asphalt containing R has a better
known fact that effect of the regenerative agents on various as-
phalts is also different. The objective of this paper is to conduct a 9.0
laboratory investigation on the high temperature properties of
8.0
the recovered asphalt binder rejuvenating with rejuvenator, waste A-5%R
cooking and cotton seed oil. Dynamic shear rheometer (DSR) test 7.0 A-5%O
A-5%W
and rotational viscosity test were conducted at different tempera-
(kPa)

6.0 A-10%R
tures on the rejuvenating asphalt to determine the rutting resis- A-10%O
5.0
tance factor, phase angle, complex modulus, failure temperature A-10%W
G*/sin

4.0 PG64-22
and rotational viscosity.
3.0

2.0
2. Experimental process and materials 1.0

Three sources of aged asphalts (referred to as A, B, and C) recovered from RAP 0.0
46 52 58 64 70 76
materials were used to blend with one type of virgin asphalt (PG 64-22) and three
percentages (0%, 5%, and 10%) of rejuvenator, cotton seed oil, and waste cooking oil Temperature ( )
(referred to as R, O, and W). The mass ratio of recovered aged asphalt to virgin as-
phalt is 1:3. Table 1 shows that G/sin d and failure temperature values of recovered Fig. 1a. G/sin d values vs. temperature for rejuvenating asphalt A with different
and virgin asphalt binders. It can be observed that the recovered binder B has the contents of R, O or W.
12 M. Chen et al. / Construction and Building Materials 59 (2014) 10–16

14.0 14.0
B-5%R
12.0 12.0 A-5%R
B-5%R B-5%O
B-5%O C-5%R
10.0 B-5%W 10.0

(kPa)
B-5%W
(kPa)

B-10%R C-5%W
8.0 B-10%O 8.0 C-5%O
B-10%W A-5%O

G*/sin
PG64-22 6.0 A-5%W
G*/sin

6.0 PG64-22

4.0 4.0

2.0 2.0

0.0
0.0 46 52 58 64 70 76
46 52 58 64 70 76
Temperature ( )
Temperature ( )
 Fig. 2a. G/sin d values vs. temperature for rejuvenating asphalt with 5%R, 5%O or
Fig. 1b. G /sin d values vs. temperature for rejuvenating asphalt B with different
5%W.
contents of R, O or W.

8.0
7.0
7.0 B-10%R
C-5%R 6.0 A-10%R
6.0 C-5%W C-10%R
C-5%O B-10%O

(kPa)
5.0
(kPa)

5.0 C-10%R C-10%O


C-10%O A-10%O
C-10%W 4.0 B-10%W
4.0
G*/sin
G*/sin

PG64-22 C-10%W
3.0 A-10%W
3.0 PG64-22

2.0 2.0

1.0 1.0

0.0 0.0
46 52 58 64 70 76 50 56 62 68 74
Temperature ( ) Temperature ( )

Fig. 1c. G/sin d values vs. temperature for rejuvenating asphalt C with different Fig. 2b. G/sin d values vs. temperature for rejuvenating asphalt with 10%R, 10%O or
contents of R, O or W. 10%W.

rutting resistance than asphalt containing W or O. In addition, the


G/sin d values of the regenerative asphalt containing 5%W are Fig. 3 shows the influences of the amount of R, O or W on the
slightly higher than the ones with 10%R at the same test tempera- phase angle. It was observed that the phase angle strongly depends
tures. In addition, the asphalts containing 5%W have close G/sin d on the amount of R, O or W and test temperatures. Generally, the
values with those with 5%O and virgin binder (PG 64-22) at the phase angle of the binders increases with an increase of the test
same test temperatures, 5%W and O can be seen as an optimum temperatures and the addition of R, O or W. The regenerative as-
dosage to produce PG 64 binder from selected aged binders. phalts containing R shows lower phase angles than the ones con-
Figs. 1a and 1c show that the rutting resistance factors of the as- taining W or O at the same condition. Thus, the elastic recovery
phalts A or C containing 5%R, 5%O or 5%W were slightly lower than performance of asphalt with R is better than asphalt containing
1.0 kPa at a temperature range from 64 °C to 70 °C. Fig. 1b shows W or O. In addition, the phase angle of the regenerative asphalt
that the asphalt B containing 10%R, 5%O or 5%W has similar trends. containing 5%W is slightly lower than the ones with 10%R. Addi-
Thus, the content of W or O is generally a small amount. tionally, the regenerative asphalt containing 5%O has slightly lower
Fig. 2 shows the effect of the regenerative agent on the rutting the phase angle than the ones with 5%W. Moreover, these rejuve-
resistance factors of two contents of three rejuvenators with three nated asphalts have close phase angles with PG 64-22 binder.
aged asphalts. For example, under an identical condition, asphalt A Fig. 4 shows the effect of three aged binder resources and three
containing 5% or 10%W shows a lower rutting resistance factor contents of rejuvenators. For example, asphalt B containing 5% or
than asphalt C. In addition, asphalt C containing 5% or 10%W shows 10%W showed a lower phase angle than asphalt C while asphalt
a lower rutting resistance factor than asphalt B. Thus, the rutting C containing 5% or 10%W showed a lower phase angle than asphalt
resistance of asphalt B containing W is the best. Similarly it can A. Thus, the elastic recovery ability of asphalt A containing W was
be noted that asphalt B containing R has the highest G/sin d values the best amongst three rejuvenated asphalts. Similar trends can be
in this study. Obviously, the resources of recovered aged binders obtained from asphalt A containing R. Obviously, Phase angle
and types of rejuvenators play an important role in determining values of these rejuvenated asphalts is noticeably dependent on
the rutting resistance of rejuvenated asphalts. the rejuvenator type and aged binder resource.

3.2. Phase angle 3.3. Complex modulus

The phase angle is defined as the time lag between shear strain G is dynamic shear complex modulus and it is the reciprocal of
and shear stress; hence it reflects the viscous response of the dynamic shear complex compliances. G is defined as the ratio of
asphalt. Generally, asphalt having a smaller phase angle has a maximum (shear) stress to maximum strain and it provides a mea-
better elastic recovery performance [21]. sure of the total resistance to deformation during shear loading.
M. Chen et al. / Construction and Building Materials 59 (2014) 10–16 13

10000 88

86
8000

Complex Modulus (Pa)


A-10%W
84

Phase Angle (Deg)


A-10%O
6000
82
A-10%R

A-5%W 80
4000
A-5%O
78
A-5%R
2000
PG64-22 76

0 74
50 52 54 56 58 60 62 64 66 68 70 72
Temperature ( )

Fig. 3a. G and d values vs. temperature for rejuvenating asphalt A with different contents of R, O or W.

14000 88

12000 86
Complex Modulus (Pa)

10000 84
B-10%W

Phase Angle (Deg)


B-10%O
8000 82
B-10%R

6000 B-5%W 80
B-5%O

4000 78
B-5%R

PG64-22
2000 76

0 74
50 52 54 56 58 60 62 64 66 68 70 72 74 76 78
Temperature ( )

Fig. 3b. G and d values vs. temperature for rejuvenating asphalt B with different contents of R, O or W.

10000 88

86
Complex Modulus (Pa)

8000
PG64-22
84
Phase Angle (Deg)

C-10%W
6000
82
C-10%O

C-10%R
80
4000
C-5%W

C-5%R
78

2000
C-5%O
76

0 74
50 52 54 56 58 60 62 64 66 68 70 72
Temperature ( )

Fig. 3c. G and d values vs. temperature for rejuvenating asphalt C with different contents of R, O or W.

Asphalt that has a large complex modulus has a better resistance to temperatures. The regenerative asphalt containing W or O shows
flow deformation. a lower complex modulus than the ones containing R at the same
Fig. 4 shows the influences of the R or O or W content on the condition. Thus, the resistance to flow deformation of the asphalt
complex modulus. Generally, the complex modulus of the binders containing R was better than the asphalt containing W or O.
decreases with an increase of the test temperatures and the Fig. 4 shows the effect of the three aged binder resources and three
addition of R or O or W. It was observed that the complex modulus rejuvenators on complex modulus. For example, Similar to rutting
strongly depends on the percentage of R or O or W and test resistance factor and phase angle, asphalt B containing rejuvenator
14 M. Chen et al. / Construction and Building Materials 59 (2014) 10–16

14000 88

12000 86

Complex Modulus (Pa)


10000 B-5%R 84

Phase Angle (Deg)


A-5%R

8000 B-5%O 82
C-5%R

6000 B-5%W 80
C-5%W

4000 A-5%O 78
C-5%O

A-5%W
2000 76
PG64-22

0 74
50 52 54 56 58 60 62 64 66 68 70 72 74 76 78
Temperature ( )

Fig. 4a. G and d values vs. temperature for rejuvenating asphalt with 5%R, 5%O or 5%W.

7000 88

6000 86
Complex Modulus (Pa)

C-10%R
5000 84

Phase Angle (Deg)


B-10%O

B-10%R
4000 B-10%W
82

C-10%W
3000 C-10%O 80
A-10%R

2000 A-10%W 78
A-10%O

PG64-22
1000 76

0 74
50 52 54 56 58 60 62 64 66 68 70 72
temperature ( )

Fig. 4b. G and d values vs. temperature for rejuvenating asphalt with 10%R, 10%O or 10%W.

100.0 0% 2.4
5%W
94.0
Pass fail temperature ( )

5%R
2.0
Rotiopnal viscosity (Pa.s)

5%O
88.0 A-5%O A-5%W
10%W
1.6
82.0 10%R
10%O A-5%R PG64-22
76.0 1.2

70.0
0.8
64.0
0.4
58.0

52.0 0.0
A B C 105 120 135 150 165 180
Asphalt binder type Temperature ( )
Fig. 5. Failed temperatures of asphalt binders. Fig. 6a. Regression analysis of rational viscosity and temperature of rejuvenating
asphalt A with R, O or W.
have the highest resistance to flow deformation. In addition, as-
phalt resource and rejuvenator type can remarkably affect the G of time–temperature equivalence principle. If the failure tempera-
value in this study. ture is high, it is more difficult to yield a permanent deformation of
asphalt concrete. In other words, when asphalt has an increase in
3.4. Failed temperature failure temperature, the rutting resistance of the mixtures will be
improved. Generally, it is similar to G/sin d.
There is a critical temperature when mixture above or below Fig. 5 shows that the influence of the amount of R, O or W on the
this temperature, time–temperature equivalence principle is no failure temperature of different binders. It was observed that the
longer applicable, and this temperature is called failure temperature failure temperature of the rejuvenated binders strongly depend
M. Chen et al. / Construction and Building Materials 59 (2014) 10–16 15

2.0 it can be pumped and handled at the hot mixing facility; also to
determine the mixing and compacting temperatures of asphalt
mixtures. In order to study the effect of various temperatures on
Rotiopnal viscosity (Pa.s)

1.6
PG64-22 B-5%W
different rejuvenated asphalts, the viscosity-temperature curves
B-7%O B-10%R were developed and regression analysis were conducted as shown
1.2
in Fig. 6 and Table 2.
Generally, as expected, the viscosity of the rejuvenated binders
0.8 decreases as test temperature increases. In this study, the viscos-
ity–temperature curves conform to a power function, and all coef-
0.4 ficients of determination values are 0.99 or higher. The relationship
can be expressed y = CxD. In the equation, y is rotational viscosity, x
0.0 is temperature, C and D are regression coefficients. The viscosity
105 120 135 150 165 180 value increases as the C increases. The regression coefficient D
Temperature ( ) reflects temperature susceptibility of asphalt. The temperature
susceptibility improved as the jDj increased. C and jDj of Table 2
Fig. 6b. Regression analysis of rational viscosity and temperature of rejuvenating
shows that asphalt A containing 5%R or 5%O or 5%W has an increase
asphalt B with R, O or W.
in the viscosity compared with PG 64-22 binder, but the effect of R
was not obvious. Asphalt B containing 10%R or 7%O or 5%W has a
2.0 lower viscosity compared with PG 64-22 binder, but the effect of
W was not obvious. Compared to PG 64-22 binder, the viscosity
of asphalt C containing 5%R or 5%W was reduced. In a word,
Rotiopnal viscosity (Pa.s)

1.6
C-5%R C-5%O additional R, O and W can slightly reduce the viscosity value of
PG64-22 C-5%W
the rejuvenated asphalt and thus decrease the mixing and compac-
1.2 tion temperatures of the mixture.

0.8 4. Conclusions

0.4 Based on the test results from three types of aged asphalt bind-
ers and three rejuvenate agents in terms of a series of conventional
and specific tests, the following conclusions can be drawn:
0.0
105 120 135 150 165 180
Temperature ( ) (1) The addition of R or O or W reduced the rutting resistance
factor of the rejuvenated asphalt binder regardless of aged
Fig. 6c. Regression analysis of rational viscosity and temperature of rejuvenating binder sources. Under the same condition, the rutting resis-
asphalt C with R, O or W. tance of asphalt containing R was better than that of asphalt
on the R, O or W contents. Generally, their failure temperature de- containing W or O. The regenerative asphalt containing 5%W
crease as the addition of R, O or W. The rejuvenated asphalts con- or 5%O could significantly decrease the rutting resistance
taining W or O show lower failure temperature values than those factor of aging asphalt to the value of virgin asphalt.
asphalts with the same content of R. Thus, under the same condi- (2) The phase angles of binders increased due to the addition of
tion, the asphalt containing R has a higher failure temperature than R or O or W. Under the same condition, the elastic recovery
asphalt containing W or O. In addition, the asphalts containing performance of asphalt with R was better than that of
5%W have close failure temperature values with the asphalt with asphalt with W or O. The regenerative asphalt containing
5%O, rejuvenated asphalts with 10%R and virgin binder (PG 64- 5%W could noticeably increase the phase angle of aged
22), but the failure temperature values of the regenerative asphalt asphalt compared with R or O.
containing 5%W are slightly higher than the same kind of rejuve- (3) The complex modulus of binders decreased due to the addi-
nated asphalts with 10%R. 5%W and 5%O can be seen as an opti- tion of R or O or W. In addition, the resistance to flow defor-
mum dosage to produce PG 64 binder from selected aged binders. mation of the asphalt containing R was better than that of
the asphalt containing W or O. The regenerative asphalt con-
taining 5%W or O could remarkably decrease the complex
3.5. Rotational viscosity modulus of aged asphalt compared with rejuvenator.
(4) Generally, the failure temperature decrease as the addition
The viscosity of an asphalt binder was used to determine the of R, O or W. The regenerative asphalt containing 5%W or
flow characteristics of the binder to provide some assurance that

Table 2
Viscosity and temperature regression analysis.

Asphalt type 120 °C (Pa s) 135 °C (Pa s) 150 °C (Pa s) 165 °C (Pa s) Regression equation Coefficient of determination (R2)
6.919
PG64-22 1.528 0.648 0.313 0.169 y = 4E + 14x 0.993
A-5%R 1.640 0.684 0.328 0.178 y = 6E + 14x6.994 0.999
A-5%W 2.016 0.788 0.378 0.208 y = 1E + 15x7.133 0.997
A-5%O 2.054 0.848 0.400 0.213 y = 1E + 15x7.134 0.9993
B-10%R 1.043 0.457 0.228 0.142 y = 1E + 13x6.323 0.9949
B-5%W 1.485 0.632 0.306 0.165 y = 3E + 14x6.906 0.9994
B-7%O 1.360 0.625 0.444 0.302 y = 5E + 09x4.61 0.9743
C-5%R 1.773 0.758 0.489 0.275 y = 1E + 12x5.693 0.9894
C-5%W 1.301 0.569 0.284 0.158 y = 8E + 13x6.636 0.9992
C-5%O 1.628 0.688 0.332 0.179 y = 4E + 14x6.937 0.9993
16 M. Chen et al. / Construction and Building Materials 59 (2014) 10–16

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