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Evaluation and Classification of Recycling Agents for Asphalt Binders

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DOI: 10.1016/j.conbuildmat.2020.119864

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 Construction and Building Materials 260 (2020) 119864

Contents lists available at ScienceDirect

Construction and Building Materials

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

Evaluation and classification of recycling agents for asphalt binders

Akash Bajaj a,⇑, Amy Epps Martin b, Gayle King c, Charles Glover d, Fawaz Kaseer e,
Edith Arámbula-Mercado f
a
Applied Research Associates, 3605 Hartzdale Dr, Camp Hill, PA 17011, USA
b
Zachry Department of Civil Engineering, Texas A&M University, College Station, TX 3136 TAMU, USA
c
GHK Inc., 10327 FM 3005, Unit 5PH1, Galveston, TX 77554, USA
d
Artie McFerrin Department of Chemical Engineering, Texas A&M University, College Station, TX 3122 TAMU, USA
e
Florida Department of Transportation, State Materials Office, 5007 N.E. 39th Avenue, Gainesville, FL 32609 USA
f
Texas A&M Transportation Institute, 1111 RELLIS Parkway, Bryan, TX 77807, USA

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

Article history: The economic and environmental benefits of using recycled asphalt materials continue to motivate agen-
Received 28 December 2019 cies to increase their proportion in new pavement construction and maintenance and rehabilitation activ-
Received in revised form 21 May 2020 ities, but the resulting reduced cracking resistance remains an engineering performance challenge. The
Accepted 4 June 2020
addition of recycling agents is one of the strategies to mitigate this issue caused by the increased stiffness
Available online 28 June 2020
and brittleness of the recycled mixture. This study explored the mechanism by which different types of
recycling agents partially restore flexibility and ductility of asphalt binder and mixtures. A binder blend
Keywords:
with 50% reclaimed asphalt pavement (RAP) binder was rejuvenated with seven types of recycling agents.
Asphalt
Binder
Rheological and chemical tools were used to evaluate the binder blends and compare their performance
Aging to a control blend without a rejuvenator to study the rejuvenation mechanism. Corresponding asphalt
Reclaimed asphalt pavement mixtures were also tested to ensure adequate performance. Based on the results, the recycling agents
Rejuvenation were divided into three categories: (a) Softeners, (b) Replenishers, and (c) Emulsifiers. The results showed
Recycling agents that while some agents act only on a physical level, others interact with the blend at a chemical level that
Rejuvenators affects the physical properties. A novel parameter was developed to compare the effectiveness of various
recycling agents.
Ó 2020 Elsevier Ltd. All rights reserved.

1. Introduction reducing energy consumption and greenhouse gas emissions and

Over 90% of pavements in the United States (U.S.) are surfaced
with asphalt mixtures. The costs of virgin materials for construc-
tion of these pavements constitute a significant share of the total
budget for these projects. The use of recycled asphalt materials
to replace the more expensive virgin materials has therefore stea-
dily increased. Around 76.2 million tons or Reclaimed Asphalt
Pavement (RAP) and 950,000 tons of Recycled Asphalt Shingles
(RAS) which includes both Tear Off Asphalt Shingles (TOAS) and
Manufactured Waste Asphalt Shingles (MWAS) were recycled in
2017, representing a savings of more than 2 billion dollars to the
asphalt paving industry [1]
In addition to the economic benefits, the use of these recycled
asphalt materials also reduces the use of virgin materials, thereby
⇑ Corresponding author.
E-mail addresses: abajaj@ara.com (A. Bajaj), a-eppsmartin@tamu.edu (A. Epps
Martin), gking@asphaltscience.com (G. King), c-glover@tamu.edu (C. Glover),
fawaz.kaseer@dot.state.fl.us (F. Kaseer), e-arambula@tti.tamu.edu (Edith Arámbula-
Mercado).
providing a sustainable method for their proper disposal. Their
inclusion in asphalt mixtures also improves performance in some
cases by enhancing the rutting resistance of pavements due to
increased stiffness. However, there are also disadvantages if the
proportions of RAP and/or RAS are too high or unbalanced. RAP
and RAS are heavily oxidized materials that have aged in the field
over a period of years. Oxidative aging in asphalt materials leads to
an increase in both stiffness and brittleness [2,3] that affects pave-
ment performance. The increased stiffness is beneficial in the short
term against rutting, but in the long term can induce cracking
when compared with virgin mixtures [4–6]. This leads many state
Departments of Transportation (DOTs) to limit the amount of recy-
cled asphalt materials in asphalt mixtures in order to balance both
short-term and long-term performance.
Different strategies have been suggested in order to mitigate
the increased stiffness and brittleness of recycled mixtures and
therefore facilitate their increased use as a replacement for virgin
materials. Use of a softer base binder with a lower performance
grade (PG) can compensate for the high stiffness and brittleness

https://doi.org/10.1016/j.conbuildmat.2020.119864
0950-0618/Ó 2020 Elsevier Ltd. All rights reserved.
2 A. Bajaj et al. / Construction and Building Materials 260 (2020) 119864

of RAP and/or RAS at relatively low proportions currently allowed
by state DOTs [7]. At relatively high proportions greater than 0.3
Recycled Binder Ratio (RBR), defined as the percentage by weight
of total recycled binder from RAP and/or RAS to total binder weight
in the binder blend or mixture, the use of a recycling agent is
required [8,9]. There are many different types of recycling agents,
and current guidance suggested by the National Center for Asphalt
Technology [10] suggested classifying them by chemistry as shown
in Table 1, but little information is provided as to the mechanism of
rejuvenation for each category.
2. Objectives and scope of work
This study was focused on understanding the mechanisms by
which different types of recycling agents improve the performance
of recycled binder blends and mixtures both initially and with
aging. Rheological characterization via Dynamic Shear Rheometer
(DSR) and chemical assessment via Fourier Transform Infrared
Spectroscopy (FTIR) were used to evaluate the recycling agents
and binder blends, and performance testing via Hamburg Wheel-
Tracking Test (HWTT) And Illinois Flexibility Index Test (I-FIT) of
corresponding asphalt mixtures was completed to ensure adequate
and balanced rutting and cracking performance.
3. Materials and methodology
The testing plan developed for this study is shown in Table 2.
The experiment was completed in three phases: (I) recycling
agents, (II) binder blends (blends with virgin materials, recycled
materials and recycling agents if added) and (III) asphalt mixtures.
The base binder and RAP used were obtained from a Port Penn/
Pole Bridge road overlay project done by DelDOT and constructed
in Fall 2016. The base binder used was a PG 64-28 unmodified bin-
der, commonly used in the region. The virgin aggregates were
obtained from an asphalt mix plant located on the southeast side
of Wilmington, Delaware. The RAP was obtained from several sec-
tions of highway in Delaware. An RBR of 0.5 was chosen to incor-
porate a high recycled materials content in the binder blends and
corresponding mixtures that could highlight the effects of recy-
cling agents. Seven types of recycling agents were chosen for the

Table 1
Types of Pavement Rejuvenators by NCAT (2014).

Category Examples Description

Paraffinic Oils Waste Engine Oil (WEO) Refined used lubricating oils
Waste Engine Oil Bottoms (WEOB)
Valero VP165Ò
StorbitÒ
Aromatic Extracts HydroleneÒ Refined crude oil products with polar aromatic oil components
ReclamiteÒ
Cyclogen LÒ
ValAro 130AÒ
Napthenic Oils SonneWarmix RJTM Engineered hydrocarbons for asphalt modification
Ergon HyPreneÒ
Triglycerides & Fatty Acids Waste Vegetable Oil Derived from vegetable oils
Waste Vegetable Grease
Brown Grease
Oleic Acid
Tall Oils SylvaroadTM RP1000 Paper industry by-products
HydrogeenÒ Same chemical family as liquid antistrip agents and emulsifiers

Table 2
Testing plan.

Materials combination Recycling agent Binder blend characterization* Mixture characterization*

characterization
Base RAP RBR Recycling agent Rheology Chemistry Conditioning Conditioning Rutting Cracking
binder Type sequence #1 sequence #2 resistance resistance
DSR1 FTIR1 Rheology Chemistry Rheology Chemistry HWTT2 I-FIT2,3
DSR1 FTIR1 DSR FTIR
PG 64-28 No – No RA U U
RAP
RAP 0.5 No RA U U U U
A1 U U U U U U U U
B1 U U U U U U U U
B2 U U U U U U U U
P U U U U U U U U
T1 U U U U U U U U
V2 U U U U U U U U
V3 U U U U U U U U
*
At dose to restore continuous PGH. DSR – Dynamic Shear Rheometer.
1
At Unaged, RTFO, PAV20 and PAV40. FTIR – Fourier Transform Infrared Spectroscopy.
2
At STOA. HWTT – Hamburg Wheel-Tracking Test.
3
At LTOA. I-FIT – Illinois Flexibility Index Test.
 A. Bajaj et al. / Construction and Building Materials 260 (2020) 119864 3

experiment to represent the types of products available in the sweeps on the recycled and rejuvenated binder blends at different
market. These recycling agents are proprietary products labeled aging levels for all material combinations. This sweep was per-
by generic descriptors that define their origin. Petroleum-based formed at three different temperatures of 5°, 15°, and 25 °C with
recycling agents in this study included aromatic extracts (A) that six frequency points per decade across an angular frequency range
are traditional recycling agents refined from crude oil as a by- from 0.1 to 100 rad/s. The rheological parameters, complex shear
product of lube oil processing with dominant polar aromatic oil modulus (G*) and phase angle (d), were obtained, and with using
components, and paraffinic oils (P) that are also refined as a by- RHEATM software [22] master curves were constructed for each bin-
product of lube oil processing, but may have similar performance der blend. These master curves were used to determine the Glover-
as recycled engine oil bottoms (REOBs). Bio-based recycling agents Rowe parameter (G-R) at 15 °C and 0.005 rad/s using the following
are derived from plant life rather than petroleum and in this study equation:
included tall oils (T) that are by-products of paper processing from
pine trees, vegetable oils (V) and simple derivatives such as esters, G Cos2 d
G
RParameter ¼
and other bio-based oils (B) that appear to be chemically reacted, Sind
usually to reduce impacts of oxidative aging on rheology. Based
The G-R parameter has a good correlation with the ductility of
on limited data, V1 is a vegetable oil that consists of a mixture of
the binder blend as shown by Glover et al. (2005) [23]. The input
glycerides, and V2 and V3 are engineered (modified) vegetable oils.
data used to calculate the G-R parameter was also plotted in a
B1 and B2 are reacted bio-based oils that consist of fatty amine
Black Space diagram along with thresholds for the onset of crack-
derivatives and bio solvents.
ing (180 kPa) and significant cracking (600 kPa). The Black Space
diagram plots the G* and d on the y- and x-axis, respectively, and
3.1. Phase I: Recycling agents
shows the change in these parameters with aging and
rejuvenation.
Selected recycling agents were fluid at room temperature, thus
The binder blends were also tested using FTIR spectroscopy to
traditional master curves used for binders and binder blends could
obtain an absorbance spectrum from 600 to 2000 cm
1 wavenum-
not be used. Complex viscosity was used instead as a rheological
ber at all aging levels to track the change in the spectrum. The
parameter, measured using a DSR with a 50 mm plate setting at
absorbance spectrum of the recycling agents themselves was also
a specific temperature of 15 °C and frequency of 10 rad/s. For
used to identify the type of the agent by identifying fingerprint
chemical assessment, Fourier Transform Infra-Red (FTIR) spec-
regions. For the binder blends, only carbonyl was considered due
troscopy was used to obtain an absorbance spectrum from
to the instability of sulfoxides in the neat binder at RTFO temper-
600 cm
1 to 2000 cm
1 wavenumber according to ASTM E1252
atures, which resulted in a decrease in peak/area between unaged
[11].
and RTFO aging levels. Carbonyl area (CA) was first calculated as
Both analyses were conducted at several aging levels. Short-
the area under the FTIR absorbance spectrum from 1650 cm
1 to
term aging was simulated using the Rolling Thin Film Oven aging
1820 cm
1 with an inclined baseline from 1524 cm
1 to
(RTFO) according to AASHTO T240 [12]. Long-term aging in the
1820 cm
1 as developed by Epps-Martin et al. (2020) in NCHRP
field was simulated using the Pressure Aging Vessel (PAV) for
9-58 [24]. Then, Carbonyl Area Growth (CAg), defined as the differ-
20 h according to AASHTO R28 [13]. Since 20-hour PAV can simu-
ence between the CA value at a particular aging level to that of the
late aging in the field of only 1–3 years based on recent research
unaged binder blend, was determined to account for the increase
[14], extended 40-hour PAV aging was also conducted to simulate
in carbonyl compounds without regard to the initial value that var-
a longer time period in the field and allow for comparison with
ied among the recycling agents (i.e., low initial values for P and A1
related research [15–17].
and high initial values for B1, B2, T1, V2, and V3).
Lastly, the binder blends were subjected to the following two
3.2. Phase II: Binder blends
separate conditioning sequences to explore the effects of aging
on rejuvenation:
Binder blends were prepared with the PG 64-28 base binder and
RAP binder extracted in accordance with ASTM D2172 [18] using a
 Conditioning Sequence #1: The rejuvenated binder blend was
centrifuge and recovered from the solvent trichloroethylene using
prepared by combining the base binder (PG 64-28) with RAP
ASTM D5404 [19]. As shown in Table 2, nine binder blends were
at 0.5 RBR, and one of seven recycling agents at a dose to restore
prepared. The first blend used only the base binder as a reference
the continuous PGH. Each blend was then subjected to 20-hour
for other rejuvenated blends. The recycled control blend had an
PAV aging. This sequence simulates field conditions.
RBR of 0.5 with no recycling agent added. Seven rejuvenated
 Conditioning Sequence #2: The recycled binder blend was pre-
blends were prepared with the different types of recycling agents
pared by combining the base binder (PG 64-28) and RAP at 0.5
at a dose that restored the continuous high-temperature PG
RBR. This blend was then subjected to 20–hour PAV and then
(PGH), the average seven-day maximum pavement temperature
back-blended with one of the same seven unaged recycling
(°C) in 1 °C increments, of the binder blend to that required by cli-
agents at the same dose used in conditioning sequence #1.
mate and traffic conditions in Delaware (i.e., PG 64-28) according
to the method described by Arámbula-Mercado et al. (2018) [20].
This was only completed at one aging level (20-hour PAV) due
When preparing the binder blends, the recycling agents (when
to time and equipment constraints. Both rheological and chemical
used) were added to the base binder, preheated at 160–170 °C,
analyses similar to the ones described previously were also com-
and stirred by hand using a spatula. The required amount of
pleted on the blends that were subjected to the two conditioning
extracted and recovered RAP binder was added to the resulting
sequences.
combination and again hand stirred by a spatula at the same tem-
perature to maintain the fluidity of the blend for complete mixing.
These binder blends were aged at four different aging levels: (a) 3.3. Phase III: Asphalt mixtures
Unaged, (b) RTFO aged, (c) RTFO + PAV aged for 20 h (PAV20),
and (d) RTFO + PAV aged for 40 h (PAV40). Laboratory mixed-laboratory compacted (LMLC) asphalt mix-
The DSR was used to determine the PG of the binder blends ture specimens were prepared using the materials identified previ-
according to AASHTO M320 [21], as well as perform frequency ously. Virgin aggregate was air dried at room temperature
4 A. Bajaj et al. / Construction and Building Materials 260 (2020) 119864

overnight and then mixed with RAP kept at a mixing temperature 4. Results and discussion
of 154 °C (310°F) for 2 h, prior to mixing, along with the base bin-
der. The recycling agent (when used) was first added to the base The results obtained from laboratory testing are discussed by
binder as a replacement for part of the total binder content [20] phase, followed by introduction of a parameter to combine rheo-
and then the combination was added to the heated aggregates logical characterization and chemical assessment.
and RAP and then mixed thoroughly using a mechanical mixer.
The resulting loose mix was short-term oven aged (STOA) at
4.1. Phase I: Recycling agents
135 °C (275°F) for 2 h to simulate aging during production and con-
struction. Afterward, the Superpave Gyratory Compactor (SGC) was
Complex viscosities were measured for all seven recycling
used to compact the specimens to 7.0 ± 0.5% air voids for perfor-
agents at each of four different aging levels at 15 °C and 10 rad/s
mance testing. Field aging was simulated for the specimens by
to observe the changes with recycling agent chemistry as well as
long-term oven aging (LTOA) the compacted specimens at 85 °C
the effect of oxidation. The results were plotted as shown in
(185°F) for 5 days following AASHTO R30 [25].
Fig. 1 on a logarithmic scale. The least amount of change with aging
The mixtures were evaluated for resistance to rutting and
(from unaged to PAV40) was observed for A1 (15%) and P (9%),
cracking. Rutting resistance for the mixtures was determined using
which are more chemically stable due to the absence of easily oxi-
the Hamburg Wheel-Tracking Test (HWTT) after STOA according to
dizable sites on the molecules. All the bio-based recycling agents
AASHTO T324 [26] at 50 °C (122°F) on two abutting cylindrical
were more sensitive to aging, with T1 (1.6  106 %) and V3
specimens with dimensions 150 mm  62 mm. The number of load
(1.1  105 %) being the most susceptible. These high values suggest
cycles to reach a rut depth of 12.5 mm was reported. Since DelDOT
cross-linkage reactions occur with oxidation in bio-based agents
specifications do not include HWTT thresholds, rutting thresholds
which increase the viscosity exponentially.
developed by the Illinois Department of Transportation (2016)
The chemical analyses yielded absorbance spectrums for all the
[27] were used to evaluate adequate performance with a minimum
recycling agents as shown in Fig. 2. Attention was given to the
number of cycles to a rut depth of 12.5 mm of 7500 for the PG 64-
region between wave numbers 1600–1800 cm
1 as it contains
XX binder.
most of the highly polar compounds that affect the rheological
Cracking resistance was measured after both STOA and LTOA
properties significantly as compared with other regions on the
using the Illinois Flexibility Index Test (I-FIT) according to AASHTO
spectrum. The peak near 1700 cm
1 is likely indicative of the pres-
TP124 [28] at 25 °C (77°F) based on successful use in previous
ence of fatty acids while the peak at 1743 cm
1 is usually due to
studies for recycled and rejuvenated mixtures [29,30,15]. Cylindri-
esters and glycerides. The presence of unsaturated sites which
cal specimens (150 mm  61 mm) were cut in half to create semi-
are more easily oxidized might explain the higher affinity for aging
circular samples, and a notch was cut at the axis of symmetry
that all bio-based agents exhibited, with T1 and V3 changing from
1.5 mm wide and 15 mm deep. Using a three-point bending config-
a fluid to almost a resin-like state after aging, suggesting some
uration, a load was applied at the rate of 50 mm/min along the ver-
association and/or crosslinking reactions taking place. The absence
tical radius until failure. The flexibility index (FI) for each specimen
of these unsaturated sites in other agents might be due to a resis-
was calculated using the following equation:
tance to aging either naturally or by modification during the man-
ufacturing process. While only one aging level is shown in Fig. 2,
similar relative results were obtained for the other aging levels.
GF
FI ¼  0:01
m 4.2. Phase II: Binder blends

The highest recycling agent dose was required for petroleum-

where GF is the fracture energy (Work of Fracture/Ligament Area) in
J/m2 and m is the slope at inflection point of the post peak load ver-
sus displacement curve. The thresholds for the test were defined by
Al-Qadi et al. (2015) at FI = 7 [29].
based recycling agents A1 and P at 13% and 11%, respectively.
The bio-based recycling agents B2 (10.5%), V2 (9%), T1 (8.5%) and
B1 and V3 (8% each) required lower doses which was concurrent
with the findings of Zaumanis et al. (2014) [31] and Kaseer et al.
(2018) [32].

Fig. 1. Complex viscosity of recycling agents with aging at 15 °C and 10 rad/s.

 A. Bajaj et al. / Construction and Building Materials 260 (2020) 119864 5

A1 (Unaged) B1 (Unaged) B2 (Unaged)

P (Unaged) T1 (Unaged) V2 (Unaged)
V3 (Unaged)
0.3

0.25
Absorbance (a.u.)

0.2

0.15

0.1

0.05

0
600 800 1000 1200 1400 1600 1800 2000
Wavenumber (cm-1)
Fig. 2. Absorbance spectra for unaged recycling agents.

Fig. 3. Black space diagram for different binder blends.

The Black Space Diagram for the binder blends is shown in Fig. 3
for the three aging levels. These values were then used to calculate
the G-R parameter for the various binder blends at different aging
levels for additional comparison. Data points in the lower right
region of the Black Space Diagram indicate low stiffness (G*) and
high ductility (d), yielding a relatively low G-R parameter. With
aging, these values would move to the upper left region of the dia-
gram with increased stiffness (G*) and brittleness (d). The diagram
also includes performance thresholds indicated by hashed and
solid lines that define a Transition Zone between the onset and
6 A. Bajaj et al. / Construction and Building Materials 260 (2020) 119864
progression of age-related block cracking in the field that is associ-
ated with G-R parameters equal to 180 kPa and 600 kPa,
respectively.
Using the base binder as a reference, the recycled blend had a
higher G-R parameter since the added RAP made it stiffer. The
addition of recycling agents to this blend at the optimum dose
for each recycling agent decreased the stiffness in all cases. How-
ever, the decrease in stiffness for binder blends rejuvenated by P
was not accompanied by an increase in phase angle. This was
attributed to the fact that P softened the recycled blend through
only physical processes. P was therefore categorized as a softening
agent like recycled engine oil bottoms. As described in Kaseer el al.
(2019) [33], softening agents are clearly aimed at lowering only the
viscosity of aged binders, while recycling agents are added to
restore the physical and chemical properties of the aged binders,
by restoring the asphaltene/maltene ratio. As seen in the absor-
bance spectrum (Fig. 2), P lacks any polar compounds which made
it highly resistant to oxidation but also increased the incompatibil-
ity with the aromatic asphaltenes and non-polar non-aromatic
paraffins present in the rejuvenated binder blends. This supports
not using paraffinic oils as asphalt binder additives as excess paraf-
finic concentrations may accelerate cracking even when aliphatic
molecules might be non-crystalline at low temperature. Recycling
agent P was chosen despite knowing this industry practice to serve
as a poor recycling agent for comparison.
A1 is a petroleum-based recycling agent that was developed
when asphalt pavement recycling began in earnest in response to
the Oil Embargo and continues to be used today. It partially
replaces aromatics and resins in binder blends lost to oxidative
aging, and is highly compatible with asphaltenes unlike paraffinic
oil P. The aromatics present also help in breaking up large asphal-
tene clusters to some extent. However, the rejuvenating properties
of A1 are dependent on the properties of the base binder and recy-
cled material, and the economics of the generally higher doses
need to be considered.
The remaining bio-based recycling agents indicate the presence
of highly polar compounds which may help in breaking large
asphaltene clusters present in the recycled materials into smaller
clusters by polarizing them and compatibilizing these smaller clus-
ters in the maltene phase. These polar compounds include fatty
Fig. 4. Absorbance spectra for unaged binder blends in carbonyl region.
acids for T1, a mixture of glycerides for V2 and V3 and glycerides
stabilized through cross linking or ester and amide bonds for B1
and B2 [34]. Therefore, these agents act more like emulsifiers for
the binder colloid system.
One notable difference between the recycling agent characteri-
zation and binder blend characterization was observed for the V3
recycling agent. T1 was susceptible to aging both alone as well as
in a binder blend, with the largest change in position on the Black
Space Diagram with aging for bio-based recycling agents; but aging
susceptibility for V3 all but disappeared in the corresponding bin-
der blend. This suggests that oxidation of recycling agents in bin-
der blends can affect the aging process. Natural antioxidants like
phenols which are present in asphalt binder [35] might not have
been strong enough to prevent oxidation of the binder itself but
might have been able to prevent oxidation of these recycling
agents by preserving their olefinic double bonds. This suggests that
evaluation of recycling agents in binder blends or corresponding
asphalt mixtures, to encompass interactions between recycling
agent and binder, is required for accurate characterization.
The FTIR absorbance for all prepared unaged binder blends is
shown in Fig. 4. The spectra are shown only for binder blends in
the carbonyl region (1650–1820 cm
1 wavenumbers) as this
region is known to be associated with important compounds in
binders and shows correlation with aging characteristics for bin-
ders [23,36–38].
As seen previously, the recycling agents contain highly polar
compounds that were detected in the carbonyl region. This led to
higher peaks in the carbonyl region when compared with the base
binder as seen in Fig. 4. These compounds might also shift peaks in
the carbonyl region due to their own chemistry. Attributing the
changes in binder blend spectra after aging to just binder oxidation
or recycling agent oxidation proved to be a difficult task. The oxi-
dized carbonyl ketones in asphalt absorbed IR light near
1700 cm
1 and the fatty acids absorbed near 1710 cm
1, causing
peaks to overlap with carbonyl peaks from asphalt oxidation.
Therefore, traditional tools like CA proved inaccurate for analyzing
rejuvenated binder blends due to the presence of carbonyl-rich
compounds in the recycling agents themselves. To overcome this
obstacle, CA growth (CAg) was utilized and plotted for different
binder blends as shown in Fig. 5.
 A. Bajaj et al. / Construction and Building Materials 260 (2020) 119864 7

Fig. 5. Carbonyl area growth for different binder blends.

The rejuvenated binder blends with bio-based recycling gents
(B’s, V’s & T1) exhibited higher CAg values than petroleum-based
recycling agents (A1 & P). These higher values for bio-based agents
can be attributed to the presence of carbonyl-rich groups like
esters, fatty acids and ketones. Normally the rheological properties
of a base binder correlate well to CAg with aging, but in the pres-
ence of recycling agents it becomes difficult to differentiate
between the CAg due to asphalt oxidation and that due to the pres-
ence of carbonyl-rich groups. Hence, traditional tools don’t capture
these differences. In addition, even though the lowest CAg amongst
the rejuvenated blends was attained by P, it only restores flexibility
(softens) when compared with other recycling agents that also par-
tially restore ductility.
Finally, the results for the conditioning sequence experiment
were analyzed. Fig. 6 shows the rheological data obtained in the
G-R Black Space Diagram for the various blends. Conditioning
sequence #1 is depicted by movement to the lower right of the dia-
gram due to rejuvenation and then a shift to the upper left due to
aging. Conditioning sequence #2 starts with movement to the
upper left in the diagram due to aging and then a shift to the lower
right due to rejuvenation. For all the cases, the binder blends that
underwent conditioning sequence #1 had a lower G* and higher d
than the corresponding ones that underwent conditioning

Fig. 6. Black space diagram for binder blends undergoing different conditioning sequences.
8 A. Bajaj et al. / Construction and Building Materials 260 (2020) 119864
sequence #2 even though aging of recycling agents occurred in
sequence #1. The G-R parameter values for sequence #2 were
almost double than for their counterparts that underwent
sequence #1 despite the use of unaged recycling agents through-
out the conditioning. This suggests that aging the recycling agents
(in sequence #1) either enhances interactions with the aged bin-
ders in a way that reduces the rheological impact of binder oxida-
tion or perhaps the presence of the recycling agents inhibits
oxidative aging of the binders. When comparing the recycling
agents, binder blends with all five bio-based recycling agents had
lower G-R parameter values within the range of 11–16 kPa for
sequence #1, while the blend with aromatic extract A1 had a
higher value (22 kPa), and the blend with paraffinic oil P exhibited
an even higher value (53 kPa).
The CAg values measured for the conditioning experiment are
reported in Fig. 7. These results indicate more oxygen uptake for
blends that underwent conditioning sequence #1. However, the
blends that underwent conditioning sequence #2 exhibited higher
G-R parameter values. These results remain true for both
petroleum-based agents, that age similarly to binders, as well as
bio-based agents. One reason for this disparity might be attributed
to the fact that oxygen diffusion through binder blends might be
different for the two sequences. Binder blends that underwent
sequence #1 were much softer and less brittle, hence oxygen diffu-
sion would be higher. However, this alone would not be able to
explain the differences in the rheology between the conditioning
sequences. These differences might also arise due to the presence
of recycling agents during aging of a binder blend. The presence
of recycling agents might divert some of the oxygen uptake to reac-
tions where the highly damaging benzylic carbonyl compounds are
not formed. These recycling agents would therefore reduce the
damaging impact of each carbonyl-based oxygen, which would
suggest additional benefits beyond the initial impact of rheology.
4.3. Phase III: Asphalt mixtures
The results from the HWTT for rutting are plotted in Fig. 8. The
recycled asphalt mixture with just RAP was the stiffest, which was
attributed to the high RAP content. Most of the rejuvenated mix-
tures passed the threshold of a minimum 7500 cycles (shown by
the red line in Fig. 8) before reaching 12.5 mm rut depth. The only
Fig. 7. Carbonyl area growth for binder blends undergoing different conditioning sequences.
rejuvenated mixture that failed to pass this threshold was the mix-
ture with P, where the incompatible nature of the recycling agent
with the asphalt binder led to high moisture susceptibility as seen
in the sharp slope after the inflection point in Fig. 8. This further
highlight the disadvantages of using an incompatible recycling
agent.
The bio-based recycling agents also displayed a trend of higher
rutting resistance with lower recycling agent dose, with the
asphalt mixture with B1 having the lowest dose and the highest
rutting resistance. The petroleum-based A1 is highly compatible
with asphalt with a lower oil content as compared to the bio-
based agents, but a higher dose is required for rejuvenation. Thus
the chemical nature of the recycling agent plays a significant role
in rutting performance of an asphalt mixture. The mixture with
B1 outperforms the mixture with V3 even though they both con-
tain the same dose of recycling agent (8%). The A1 mixture also
outperforms many other rejuvenated mixtures even though it
includes a high dose.
Comparing recycling agents with similar chemistry, asphalt
mixtures with lower doses of recycling agents, such as B1 and
V3, perform better than their counterparts that require a higher
dose (B2 and V2). This performance gap is especially visible in
the case of bio-based oils B1 and B2. These observations suggest
putting an upper limit on the dose of recycling agent to prevent
premature rutting.
The results for the I-FIT cracking test along with error bars to
represent the variability are shown in Fig. 9. As expected, the recy-
cled asphalt mixture performed the worst due to its extremely
high stiffness to the point where FI after LTOA could not be mea-
sured. This high stiffness is the primary reason to limit the amount
of recycled asphalt materials in mixtures. After STOA, the mixtures
with reacted bio-oils B1 and B2 performed the best by having the
highest FI, followed by aromatic A1, vegetable oils V2 and V3,
paraffin P and tall oil T1. After LTOA, a drop in FI was seen, as
expected, with an increase in stiffness and brittleness due to oxida-
tion. The rejuvenated mixture with B1 still performed the best, fol-
lowed by the rest of the mixtures with bio-based recycling agents.
The asphalt mixtures rejuvenated with T1 (41.4%), A1 (41.2%), and
P (41.1%) had the highest percentage decreases in FI with aging.
The poor performance of P as a rejuvenator was expected as it only
restores flexibility. As discussed, the increased aging susceptibility
 A. Bajaj et al. / Construction and Building Materials 260 (2020) 119864 9

Fig. 8. HWTT for different asphalt mixtures.

Fig. 9. I-FIT results for different asphalt mixtures.

of T1 is highlighted again as was the case with binder blends and as
a recycling agent itself. The bio-based recycling agents B1 (22.1%),
B2 (32.2%), V2 (38.2%), and V3 (18.4%) had lower percentage
decreases in FI after aging. The modified vegetable oils and reacted
bio-oils were less susceptible to aging as recycling agents as well as
in binder blends. These recycling agents were modified to make
them less susceptible to oxidation with time. Conclusions for V3
could not be drawn due to the high variability after STOA.
Even though A1 performed well in a binder blend, it showed a
significant drop in FI with aging. This can be attributed to the agent
10 A. Bajaj et al. / Construction and Building Materials 260 (2020) 119864

not being modified to make it less susceptible to aging. All asphalt
mixtures did meet the current threshold requirement for I-FIT set
at 7.0 for STOA specimens. However the newer, bio-based recycling
agents seem to be more heavily modified which makes them better
in terms of long-term performance.
4.4. Binder embrittlement parameter
Both rheological and chemical properties assessed in this study
ultimately affect the performance of binder blends and corre-
sponding mixtures. To truly compare the performance of recycling
agents, a combined parameter is needed which not only captures
the change in rheology of a binder blend with aging but also
includes the change in rheology due to oxidation measured by a
chemical parameter. The G-R parameter for various binder blends
at different aging levels was plotted on a semi-logarithmic graph
against CAg as shown in Fig. 10. A best fit line was drawn through
these points to indicate the change in G-R parameter in correlation
to the change in CAg with aging.

Fig. 10. G-R parameter vs CA growth for different binder blends with aging.

Fig. 11. Binder embrittlement parameter for different binder blends.

 A. Bajaj et al. / Construction and Building Materials 260 (2020) 119864
A new parameter called the Binder Embrittlement Parameter
(BEP) was defined as follows to combine both the G-R parameter
and CAg to capture the rheological state initially and with extended
aging and the rate of change in rheology with oxidation:
BEP ¼ Log½ðG
RRTFO  G
RPAV40 Þ  ðChange in Log G

2 i

R Parameter=Change in CAg :
The first term, G-RRTFO  G-RPAV40, is used to represent the ini-
tial and final rheological parameters. Unaged values were not used
as CAg was being tracked and unaged CA values are used as the
basis to calculate CAg for other aging levels. The second term,
Change in Log G-R Parameter/Change in CAg, a hardening suscepti-
bility, serves as the slope of the plotted graph and hence represents
the change in the rheological parameter per unit change in the
chemical parameter.
A lower value of BEP indicates a lower stiffness and increased
ductility as well as less rheological response to oxidation during
aging. Both of these qualities are desirable for the binder blend
and corresponding mixture. The BEP for various binder blends is
shown in Fig. 11. The recycled blend had a significantly
higher value than the rejuvenated blends even though it had a
low hardening susceptibility slope due to an extremely high initial
stiffness because of the large quantity of RAP and no recycling
agent. The base binder served as a control to evaluate the other
blends.
As expected, the rejuvenated blend with P did not perform as
well as the blends with other recycling agents due to both a higher
G-R parameter and a greater response to oxidation. The bio-based
recycling agents, again, proved to be the most effective with
reacted bio-oils B1 and B2 performing the best. The rankings
obtained from the BEP were consistent with those observed in
the other analyses including evaluation of the recycling agents
themselves, binder blends and asphalt mixtures.
5. Conclusions and recommendations
This study explored the rejuvenating mechanisms of different
recycling agents used in asphalt mixtures with high proportions
of recycled asphalt materials. Results were obtained by analysis
of these recycling agents themselves, in binder blends and in cor-
responding asphalt mixtures using rheological and chemical tools
and performance tests. The main findings of this study can be sum-
marized as follows:
 Testing of recycling agents by themselves may not be represen-
tative of their behavior in binder blends. The chemistry of the
recycling agents can be influenced when combined with bin-
ders; thus, binder blends should be tested for accurate
characterization.
 Recycling agents included in the study interacted with the recy-
cled materials in different ways and therefore can be classified
based on their mechanism of rejuvenation into three categories:
(a) Softener, (b) Replenisher or (c) Emulsifier.
 The paraffinic oils (P) were not expected to act as a good rejuve-
nator. They still met the PG requirements for rejuvenated bin-
der blends when an appropriate dose was added to the
recycled and base binders, but they performed poorly in almost
all of the rheological evaluations likely due to incompatibility
among the fractions, placing them in a separate category of
Softener from the other recycling agents.
 Aromatic extracts act as Replenishers to replace the aromatics
and aromatics lost to oxidation while maintaining compatibil-
ity. The one used in this study performed well under extended
aging levels like PAV40 and outperformed other petroleum-
11
based recycling agents. However, the quality of the base binder
as well as the recycled materials content could affect the rejuve-
nating capabilities of aromatic extracts, oftentimes requiring
high doses that may not be economical.
 The modified vegetable oils and reacted bio-oils were the most
effective recycling agents. Even though they lack aromatics,
these agents offered a different mechanism for rejuvenation
and can be classified as Emulsifiers with highly polar carbonyl
groups attaching themselves to asphaltenes clusters while ole-
finic chains remain mobile in the maltenes. Oxidation may lead
to a decrease in the benefits of double bonds, but the same
might not be reflected in the rheological parameters. Modifica-
tion of these agents to resist long-term aging also helps retain
their effectiveness with oxidation.
 Tall oils also contain strong polar compounds that provide a
similar rejuvenation mechanism to that for reacted bio-oils
and modified vegetable oils, so they can also be classified as
Emulsifiers, but a separate sub-category or additional category
may be needed because their unsaturated double bonds are
prone to oxidation.
 The presence of strongly polar groups in recycling agents proves
challenging for characterization using traditional tools like FTIR.
CA can increase by the presence of recycling agent, but not all
the oxygen uptake leads to an increase in the G-R parameter.
Instead, oxidative impact on key rheology indicators tied to
cracking seemed to be ameliorated for all recycling agents.
Therefore, CA was discarded in favor of CAg which measures
the growth between two aging levels to normalize this effect.
 The type and dose of recycling agents can also affect rutting per-
formance. The chemistry of a recycling agents plays a significant
role followed by the dose. Also, newer recycling agents on the
market seem to be modified more heavily to make them less
susceptible to oxidation with aging to help them retain their
cracking performance.
 Considering all of these factors, reacted bio-oils exhibited the
best performance followed closely by the modified vegetable
oils. Tall oils performed better than the petroleum-based prod-
ucts, but their aging susceptibility cast doubt on long-term
effectiveness in the field. Aromatic extracts, with better com-
patibility with asphalt binders, were more effective than paraf-
finic oil that acted only as a softening agent.
 This study was based on only one base binder and one RAP
source and RBR, so additional materials combinations need to
be characterized to explore the effectiveness of the proposed
novel BEP and its possible use in redefining the recycling agent
classification system based on mechanism and the effects of
chemistry on rheology.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
Acknowledgements
This study was performed under the National Cooperative High-
way Research Program (NCHRP) Project 09-58: The Effects of Recy-
cling Agents on Asphalt Mixtures with High RAS and RAP Binder
Ratios.
12 A. Bajaj et al. / Construction and Building Materials 260 (2020) 119864
Disclaimer
This paper does not constitute a standard, specification, nor is it
intended for design, construction, bidding, contracting, or permit
purposes. Any opinions, findings and conclusions, or recommenda-
tions expressed in this publication are those of the authors and do
not necessarily reflect the views of NCHRP.
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