Effect of Aging on the Rheological

Properties of Blends of Virgin

and Rejuvenated RA Binders

Di Wang, Augusto Cannone Falchetto, Martin Hugener, Laurent Porot,

Atsushi Kawakami, Bernhard Hofko, Andrea Grilli, Emiliano Pasquini,
Marco Pasetto, Hassan Tabatabaee, Huachun Zhai, Margarida Sá da Costa,
Hilde Soenen, Patricia Kara De Maeijer, Wim Van den Bergh,
Fabrizio Cardone, Alan Carter, Kamilla L. Vasconcelos,
Xavier Carbonneau, Aurelie Lorserie, Goran Mladenović, Marko Orešković,
Tomas Koudelka, Pavel Coufalik, Edoardo Bocci, Runhua Zhang,
Eshan V. Dave, and Gabriele Tebaldi

Abstract The use of rejuvenators has seen a consistent increase over the years in
the asphalt pavement industry. This is due to the need for maximizing the demand for
incorporating a higher amount of Reclaimed Asphalt (RA) in the pavement asphalt
mixtures. In order to tackle this challenge, the Task Group 3, focusing on asphalt

D. Wang
Technische Universität Braunschweig, Braunschweig, Germany
A. Cannone Falchetto (B)
University of Alaska Fairbanks, Fairbanks, AK, USA
e-mail: afalchetto@alaska.edu
M. Hugener
Empa—Materials Science and Technology, Dübendorf, Switzerland
L. Porot
Kraton Chemical B.V., Almere, The Netherlands
A. Kawakami
Public Works Research Institute, Tsukuba, Japan
B. Hofko
Institute of Transportation, TU Vienna, Vienna, Austria
A. Grilli
University of the Republic of San Marino, San Marino, Republic of San Marino
E. Pasquini · M. Pasetto
University of Padova, Padova, Italy
H. Tabatabaee
Cargill, Wayzata, MN, USA
H. Zhai
Idaho Asphalt Supply Inc., Idaho Falls, ID, USA
M. S. da Costa
National Laboratory of Civil Engineering (LNEC), Lisbon, Portugal

© The Author(s), under exclusive license to Springer Nature Switzerland AG 2022 3

H. Di Benedetto et al. (eds.), Proceedings of the RILEM International Symposium on
Bituminous Materials, RILEM Bookseries 27,
https://doi.org/10.1007/978-3-030-46455-4_1
4 D. Wang et al.

binders and additives, of the RILEM TC RAP conducted an interlaboratory activity to

evaluate the effect of aging on blends of virgin and rejuvenated RA binders. A set of
conventional tests including penetration value at 25 °C, softening point temperature
and rheological measurements by means of Dynamic Shear Rheometer (DSR) were
selected to involve a large number of participants. A binder, recovered from field
RA, was treated with a bio-based rejuvenator and blended with a virgin binder to
simulate recycling at three different percentages 60, 80, and 100%. These blends,
as well as the pure virgin binder, were next short and long term aged and tested to
evaluate the changes in the corresponding properties. Relatively consistent results
were obtained for the entire set of blends. The aging of combined rejuvenated RA
and virgin binders was comparable to that experienced for the pure virgin binder.
DSR data provided a more precise evolution of the impact of aging on the materials.

Keywords Asphalt binder · Reclaimed asphalt (RA) · Rejuvenator · DSR

1 Introduction

In the considerations of both environmental and economic benefits, different types of

recycled, industrial by-products materials have been used for the asphalt pavement

H. Soenen
NYNAS, Antwerp, Belgium
P. K. De Maeijer · W. Van den Bergh
University of Antwerp, Antwerp, Belgium
F. Cardone
Polytechnic University of Marche, Ancona, Italy
A. Carter
LCMB-ETS Montreal, Montreal, Canada
K. L. Vasconcelos
Laboratory of Pavement Technology—University of São Paulo, São Paulo, Brazil
X. Carbonneau · A. Lorserie
CST COLAS, Magny-les-Hameaux, France
G. Mladenović · M. Orešković
Faculty of Civil Engineering, University of Belgrade, Belgrade, Serbia
T. Koudelka · P. Coufalik
Brno University of Technology, Brno, Czech Republic
E. Bocci
eCampus University, Novedrate, Italy
R. Zhang · E. V. Dave
University of New Hampshire, Durham, NH, USA
G. Tebaldi
University of Parma, Parma, Italy
Effect of Aging on the Rheological Properties … 5

construction for several decades [1] making reclaimed asphalt pavement materials
one of the most reused construction materials [2, 3]. Different technologies can
be selected to maximize the use of the Reclaimed Asphalt (RA) within the Hot Mix
Asphalt (HMA) in a laboratory environment. However, due to the aged asphalt binder
with higher stiffness and brittleness, the reuse of a high amount of RA can lead to
potentially poorer performance of asphalt pavements against cracking [2, 4]. Hence,
the use of RA in HMA is commonly limited to 25–50% for construction purposes
[4].
In the upcoming decades, more and more RA have to be recycled and reused due to
environmental and economic reasons. The current degree of recycling undoubtedly
limits the design possibilities of pavement engineers and road authorities. Therefore,
novel technologies are needed to maximize the value of RA up to a higher level.
The use of rejuvenators represents an alternative solution to increase the rate of RA
or the use of very hard RA, minimizing the impact of the recycled material on the
performance properties of the mixtures and pavements [5]. In several previous studies
[6–8], it has been successfully demonstrated that some rejuvenators can substantially
restore the properties of aged asphalt binder with limited impact on its temperature
susceptibility.
With respect to the use of a high level of RA in asphalt pavement, RILEM estab-
lished a specific Technical Committee (TC): 264-RAP (Asphalt Pavement Recy-
cling). Within the framework of this TC, Task Group 3 on Asphalt Binder for Recy-
cled Asphalt Mixtures is devoting its activities on the investigation of the effect
of restoring the lost properties of aged RA binders by using rejuvenators. A total
of 20 laboratories have committed to participate in this group; some outcomes have
been already reported [9, 10]. This paper mainly focuses on presenting and analyzing
the results from the rheological tests.

2 Experimentation

2.1 Materials

The RA binder was extracted with Trichloroethene and recovered according to

EN 12697-1 and EN 12697-3 standard by one single laboratory, from an RA material
source collected in Germany. The selected rejuvenator was a bio-based additive; its
specific amphipathic chemical structure, disperses the highly polar fractions limiting
the agglomeration of asphaltenes [11]. A 50/70 paving grade binder (EN 12591) was
used as reference material. The proposed procedure ensures that a single source of
material can be used by all the laboratories throughout the entire research activity.
Additional information on the selected materials can be found elsewhere [10, 12].
After extraction RA binder was melted at 160 °C and blended with 8% of rejuvenator
manually mixing the blend at 160 °C for one minute. The rejuvenated binder was
tested as it is (100 RA) or with a 50/70 paving grade bitumen. The blends consisted
6 D. Wang et al.

of 60% and 80% of the rejuvenated binder and a complementary part of 50/70 which
were named 60 RA and 80 RA, respectively.

2.2 Testing Plan

The testing plan consisted of evaluating different blends of RA binder which were
treated with an optimal amount of rejuvenator and virgin binder in a ratio of 60,
80, and 100%. The optimal rejuvenator content was determined in a preliminary
study [9]. An initial analysis of basic properties confirmed that through the optimal
rejuvenator dosage it is possible to recover the penetration value of a target 50/70
fresh blend material as a function of the three different blend ratios (60 RA, 80 RA,
and 100 RA) [10]. In addition, to better evaluate the aging effect on the performance
properties of virgin binder and blended binders, artificial aging procedures were
conducted in the laboratory environment. Different studies have begun evaluating
binder durability at extended aging times (40 h of PAV aging or longer) as potentially
more indicative of binder long term performance of binders modified with additives
[13]. However, in this research, standard short and long-term aging was performed
for each material with the Rolling Thin Film Oven Test (RTFOT) and Pressure Aging
Vessel (PAV) procedures based on EN 12607-1 and EN 14769, respectively.
For each material under different aging levels, the penetration values at 25 °C (EN
1426) and the softening point temperature (EN 1427) were measured. Temperature-
frequency-sweep (T-f-sweep) tests were performed on each binder by using the
Dynamic Shear Rheometer (DSR) (EN 14770). Testing was performed at tempera-
tures, ranging between −6 and +82 °C every 6 °C, with the 4, 8 and 25 mm plates.
A frequency sweep from 0.1 to 10 Hz was used. Since 20 different laboratories from
different regions were involved in this research, each laboratory selected only a single
blending ratio among the three proposed. Among the participants, 16 laboratories
provided softening point temperature and DSR results and 11 the penetration values.

3 Results and Analysis

3.1 Penetration Value and Softening Point

As mentioned before, the use of the rejuvenator can restore the fresh blend asphalt
binder to the target properties (penetration); however, this capability may be mitigated
over time. The experimental results of the penetration value and softening point under
different aging conditions are analyzed and discussed in this section to evaluate the
aging effect of rejuvenators. As an example, the trend of the virgin and 80% blend
ratio from four laboratories under different aging conditions is shown in Fig. 1.
Effect of Aging on the Rheological Properties … 7

Fig. 1 Comparison among 50/70, 80 RA and RA binders under different aging conditions

Only limited differences can be observed among the four laboratories, while very
similar trends are found for virgin and blend materials under different aging condi-
tions. Hence, the relative change in properties is of the same order of magnitude.
This trend can be also observed in the case of 60 and 100% blend ratios. Overall, no
remarkable difference in basic properties was found between the three blend ratios
at the different aging levels highlighting the role of the rejuvenator in restoring the
consistency of blended RA binders. Results confirmed that the selected rejuvenator
dosage allows restoring the consistency of RA binder at 25 °C and high service
temperatures. It can be affirmed that the effect of aging on 80 RA is similar to that
on 50/70.

3.2 Dynamic Shear Rheometer (DSR) Results

The evolution of DSR results is reported as a function of the different aging conditions
in Figs. 2 and 3 for two different representative temperatures, 28 and 58 ºC. Results
refer to the single frequency of 1.59 Hz. As in the previous section, the 80% blend
ratio is presented as an example. The plot of complex shear modulus |G*| versus
phase angle δ under different aging conditions is exhibited. The average value and
the results from each laboratory are displayed. From Fig. 2, it can be observed that the
participating laboratories had relatively similar measurements at both temperatures
(28 and 58 ºC). For the different aging levels. Linear relationships are found between
the logarithm of the complex shear modulus |G*| and phase angle δ. Overall, the
effect of the rejuvenator in the blend ratio of 80% was preserved also at the different
aging levels, as supported by the experimental measurements of the four laboratories.
Similar results can be found in the blend ratio of 60 and 100%.
8 D. Wang et al.

Fig. 2 Complex shear modulus |G*| versus phase angle δ at a 28 ºC and b 58 ºC

A comparison among the different blends (50/70, 60 RA, 80 RA, and 100 RA)
across the three aging levels at 28 and 58 ºC was performed reporting the average
value of |G*| at 1.59 Hz in the bar charts of Fig. 3.
A non-univocal trend is observed for |G*| at the two selected temperatures. While
at 28 ºC the shear modulus of the rejuvenated material is generally lower than the
virgin one regardless of aging conditions, an opposite trend is exhibited at 58 ºC.
Further studies will investigate the rejuvenated binder properties in comparison with
50/70 over a wide range of temperatures through master curve and black diagram
analysis.

4 Conclusions

In the present study, the possibility of using rejuvenators to reuse, for the mix design
a high amount of binder obtained from RA was experimentally investigated with
the penetration grading system and DSR measurements. Based on the experimental
results and analyses the following conclusions can be drawn:
Effect of Aging on the Rheological Properties … 9

Fig. 3 Complex shear 1.E+07

modulus |G*| for virgin 60RA 80RA 100RA 50/70
binder and blends at a 28 ºC
and b 58 ºC 1.E+06

G* [Pa]
1.E+05

1.E+04

1.E+03
virgin RTFOT PAV a)
1.E+07
60RA 80RA 100RA 50/70

1.E+06
G* [Pa]

1.E+05

1.E+04

1.E+03
virgin RTFOT PAV b)

• The optimal rejuvenator dosage does not change when using different proportions
of RA and 50/70 binder. A single optimal rejuvenator content can be used to
partially restore the rheological properties at different blending ratios.
• The use of rejuvenators can contribute to the recovery of the rheological properties
of a blend of RA and virgin binders at intermediate temperatures while preserving
the benefit at high temperatures.
• Based on the standard aging procedure, the proposed DSR-graph with G* and
phase angle can be used as a general method to test the performance of a
rejuvenator in combination with an RA-binder, a virgin binder, and other additives.
Although the results obtained in this study are promising, additional experimental
support is needed by extending the present research effort to the investigation of
more types of RA binders and different rejuvenator categories, as well as potentially
extending the aging time.

Acknowledgments The RILEM Technical Committee on Asphalt Pavement Recycling (RAP) 264
and the contributions of Nynas AB, Kraton Chemical B.V. and TU Braunschweig ISBS pavement
laboratory staff to the RILEM interlaboratory activities are gratefully acknowledged.
10 D. Wang et al.

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