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Influence of rejuvenators on bitumen ageing in hot recycled asphalt mixtures

Article in Journal of Traffic and Transportation Engineering (English Edition) · June 2018
DOI: 10.1016/j.jtte.2018.01.001

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Post-print version. Published version available from:
https://doi.org/10.1016/j.jtte.2018.01.001

Original research paper

Influence of rejuvenators on bitumen

ageing in hot recycled asphalt mixtures

Giorgia Mazzonia, Edoardo Boccib,*, Francesco Canestraria

a
Università Politecnica delle Marche, Department of Civil and Construction Engineering and Architecture,

Ancona 60131, Italy

b
eCampus University, Faculty of Engineering, Novedrate (CO) 22060, Italy

Highlights

• Evaluation of bitumen service life including its reuse in hot recycling.

• Effect of different rejuvenators on the bituminous blends was analysed.

• Rejuvenated bitumens guarantee lower ageing than virgin bitumen alone.

• At the end of service life rejuvenated bitumen can be less stiff than virgin one.

Abstract

The use of reclaimed asphalt pavement (RAP) in new hot mix asphalt (HMA) by means of

hot recycling techniques generates the advantage linked to the exploitation of both lytic

and bituminous component, consequently leading to the decrease of both virgin

aggregates and bitumen supplying. However, many agencies and public administration

authorise RAP percentages ranges from 10% to 30% in hot recycling. The main reason for

such a low amount of allowable RAP content is related to the aged bitumen contained in

the RAP materials, which is more brittle than a virgin bitumen leading to a final mixture

more susceptible to fatigue, thermal and reflection cracking. The use of rejuvenators has

1
Post-print version. Published version available from:
https://doi.org/10.1016/j.jtte.2018.01.001

the potential to restore rheology and chemical components of aged RAP bitumen, thus

allowing a significant increase in the amount of RAP to be properly implemented in HMA.

The experimental investigation is described in this paper and carried out through a

dynamic shear rheometer (DSR) which provides the rheological characterisation of a

paving grade bitumen during its overall service life including its reuse in hot recycling by

adopting different rejuvenators.

Results show that rejuvenators modify bitumen chemistry and consequently rheology

by enhancing the viscous response. Moreover, it was observed that oxidation is less

harmful, in terms of stiffness increase, on the 50/50 aged bitumen - virgin bitumen blends

(rejuvenated or not) than on the virgin bitumen. Moreover, the addition of a rejuvenator in a

bituminous blend containing 50% of bitumen reactivated from RAP could lead to a

corresponding composite bituminous phase less subjected to ageing phenomena and

even less stiff at the end of service life than the associated virgin bitumen alone.

Keywords:

Rejuvenator; Reclaimed asphalt pavement; Bitumen; Ageing; Dynamic Shear Rheometer (DSR).

*Corresponding author. Tel.: +39 338 467 7744.

E-mail addresses: g.mazzoni@pm.univpm.it (G. Mazzoni),
edoardo.bocci@uniecampus.it (E. Bocci), f.canestrari@univpm.it (F. Canestrari).

2
1 Introduction

Nowadays, the implementation of high reclaimed asphalt pavement (RAP) contents in the production of

new hot mix asphalt (HMA) represents a challenging issue for highways agencies and paving

companies. The main factors that encourage the use of RAP in HMA are economic and environmental

benefits, such as reducing production costs and disposal in landfills as well as preserving natural

resources.

Although RAP has its origin from the demolition of damaged asphalt pavements, this material should

not be considered as a waste product (Karlsson and Isacsson, 2006), since the important residual

properties of bitumen and mineral aggregates contained in RAP could be profitably exploited through

hot and cold recycling techniques.

Cold recycling allows reaching the highest amount of RAP to be reused. However, since in cold mix

asphalt (CMA) RAP acts as a “black aggregate”, the low production temperature does not allow the

reactivation of RAP bitumen that hardly interacts in an efficient manner with new bitumen (Grilli et al,

2012).

As regards hot recycling technique, the use of RAP allows a double advantage through the

exploitation of both lytic and bituminous component (Al-Qadi et al., 2007), leading to a reduction of virgin

aggregates and bitumen supplying in the production of HMA. However, many agencies and public

administrations authorise low RAP percentages ranging from 10% to 30% in hot recycling, due to

different concerns.

First, the phenomena of RAP bitumen mobilisation and its blending and interaction with the new virgin

bitumen during mix production represent uncertainties which are still under investigation worldwide.

Despite the considerable efforts in characterising the interaction between virgin and RAP bitumens

(Booshehrian et al., 2013; Navaro et al., 2012; Nguyen, 2009) and their degree of blending (Bressi et al.,

2016; Frigio et al., 2015, Shirodkar et al., 2011; Stimilli et al., 2015; Yousefi Rad, 2013), only little

fundamental information is available in literature about the physicochemical phenomena and

mechanisms during the mixing of a new HMA with RAP. Inaccurate assumptions on the effects of

interaction could create problems in both mix design and pavement performance, leading to a final

3
mixture more susceptible to cracking, ravelling, moisture damage and rutting (Dondi et al., 2016;

Noferini et al., 2017; Zaumanis et al, 2014).

Moreover, a critical issue is related to the ageing process, which affects physical and chemical

characteristics of RAP bitumen entailing a general hardening of the final bituminous blend. As well

known, bitumen undergoes two different ageing phases: short- and long-term ageing. The former

represents the ageing during plant mixing, transportation and paving and is related to oxidation and

lighter components evaporation. Whereas the latter occurs during pavement service life and is mainly

linked to oxidation and physical hardening (Lu et al., 2017). Presence of water, local climate, thickness

of the bitumen film and, mostly, mix porosity represent the main factors that influence the degree of

long-term ageing.

Generally, ageing process causes a progressive change in bitumen rheological and chemical

properties, leading to a reduction of the aromatic content and a consequent increase in the amount of

resins (which in turn generate asphaltenes), whereas saturates remain essentially unchanged due to

their poor reactivity (Lesueur, 2009). Since asphaltenes play a major role in determining bitumen

viscosity, it is evident that oxidation causes a stiff behaviour (bitumen hardening) in addition to poor

adhesion and reduction of coating properties.

In addition, the maximum amount of RAP to be reused in HMA production depends not only on the

ability to correct the physicochemical characteristics of the aged bitumen, but also on the production

technology (Mogawer et al., 2012). Considering hot in plant recycling, most conventional drum plants

can accommodate 50% RAP, whereas the percentage of reusable RAP in batch plant ranges from 10%

to 30% (Kandhal et al., 1997).

When high amounts of RAP (30% or more) are introduced in the production of new HMA, the use of

specific additives is strongly recommended to achieve adequate workability and final mechanical

performance (Chen et al, 2007; Haji et al., 2013; Shen et al., 2007; Tran et al., 2017; Xie et al., 2017; Yu

et al., 2014). The additives should be non-hazardous and stable over a wide range of temperatures,

from production to application. In addition, they must not experience any exudation or evaporation, in

order to guarantee a good performance over asphalt pavement lifetime (Bocci et al., 2017; Grilli et al.,

2015).

4
 Among recycling additives, a distinction can be made between softening agents and rejuvenators.

The softening agents aim at reducing aged bitumen viscosity, whereas rejuvenators attempt to restore

the chemical and rheological properties of aged bitumen, thus ensuring long lasting HMA (Grilli et al.,

2017, Tabakovic et al., 2017). Rejuvenators can have different nature, which reflects in the molecular

structure and polarity (Zaumanis et al., 2014). In the last years, many products including tall oils, organic

oils or recycled waste oils have been used worldwide to mobilise the aged bitumen in the RAP with the

double benefit of possibly increasing RAP content in the mix and achieving good HMA performance. In

particular, it has been observed (Booshehrian et al., 2013; Oldham et al., 2018) that the same target

rheological properties, comparable to those of a virgin bitumen, can be obtained by mixing the aged

RAP bitumen with a rejuvenator. However, the chemical composition (e.g. the ratio of asphaltenes to

maltenes) of the rejuvenated binder is significantly different from that of the virgin bitumen, affecting the

long-term performance of the RAP mix (Asli et al., 2012; Shen et al., 2007; Zargar et al., 2012).

Numerous studies have been undertaken on the effect of recycling additives within aged bitumen, but

the ageing process of rejuvenated bitumen is still a challenge.

2 Objectives

The main objective of this research is the evaluation of the rheological properties of a neat paving grade

bitumen considered during its overall service life, which includes its reuse in hot recycling by adopting

different rejuvenators. To this purpose, bitumen properties have been investigated simulating different

conditions of its service life: before and after HMA production, at the end of pavement service life, during

hot recycling process, after laying of hot recycled HMA and, finally, at the end of the hot recycled HMA

service life. In detail, the following aspects have been studied:

• assessment of the ageing effects on rheological properties of the virgin bitumen selected.

• determination of the interaction among virgin and RAP bitumens with/without rejuvenator and the

related effects on the rheological properties of the corresponding composite bituminous blends.

• investigation of the ageing effects on the rejuvenated bitumens.

5
3 Materials

3.1 Bitumen

The binder selected was a 50/70 pen bitumen obtained as the residue from a visbreaking process.

Visbreaking (i.e. viscosity breaking) is a relatively mild thermal cracking process operated at

455–510 °C and 0.3-2 MPa (3*20 bars) for a short residence time (1*3 min), which allows to reduce the

viscosity of residua without attempting coke formation and significant conversion to distillates. The main

limitation of the visbreaking process is that the products can be unstable. In fact, thermal cracking at low

pressure gives olefins that, in turn, produces a very unstable material tending to undergo secondary

reactions (oxidation) to form intractable residua (Speight, 1999).

The basic properties of the reference bitumen used in this study are summarised in Table 1.

Table. 1 Basic properties of the reference bitumen used.

Code Penetration at T = 25 ℃ Softening point Penetration index Retained penetration

(dmm) (℃) (/) after RTFOT (%)

Virgin bitumen VB 62 46 – 54 -1.5 – 0.7 >50

3.2 Rejuvenators

In the present research, three commercial rejuvenators, commonly used for hot recycling, have been

chosen. The first (rejuvenator type A) is a miscible crude tall oil derived from the processing of pine

wood in paper industry, and contains fatty acids, resin acids and unsaponifiables. The second

(rejuvenator type B) is a mix of different chemicals and consists of modified polyamines and vegetal oils.

The third (rejuvenator type C) is an organic refined additive consisting of alkylates and fatty acids. The

physical characteristics of the three rejuvenators are shown in Table 2.

Table 2 Basic properties of the rejuvenators.

Density at T =20 ℃ Kinematic viscosity at T =20 ℃

Rejuvenator 3
(g/cm ) (mm2/s)
A 0.93 98
B 0.80 45
C 0.88 47

6
4 Bituminous sample preparation

Starting from the virgin bitumen and the three rejuvenators above-mentioned, fifteen bituminous blends

were artificially manufactured in laboratory to simulate the overall service life of a reference bitumen (i.e.

ageing of a bitumen within a new HMA, rejuvenation of bituminous blends within new HMA containing

high RAP content by means of three different additives and ageing of rejuvenated bitumens).

The first service life of the bitumen selected was simulated by subjecting it to a short- and long-term

ageing, by means of rolling thin film oven test (RTFOT) and pressure aging vessel (PAV) testing

procedures, in accordance with European Standards EN 12607-1 and EN 14769. In details, the RTFOT

procedure requires an electrical heated convection oven at 163 °C that contains a vertical circular

carriage to accommodate eight sample bottles covered by a film of bitumen for 85 minutes. The oven is

also equipped with an air jet that blows air in each bottle while the carriage circulates. With respect to

PAV, the equipment consists of a vessel including a cylindrical chamber with a top lid secured by means

of a shear ring assembly composed of an aluminum lock ring and bronze shear ring segments. The

chamber can accommodate ten sample pans placed in a sample rack. The combined action of

temperature, which is set equal to 100 °C, and pressure of 2.1 MPa should be able to reproduce in only

20 hours for the same effects caused by the climate agents on the pavements over a service period from

5 to 10 years.

It should be highlighted that the same aged bitumen obtained with the above-mentioned procedure

was also used to reproduce the RAP bitumen. Hot recycling was simulated by blending 50% of the virgin

bitumen, 50% of RAP bitumen and, in case, one of the three additives selected. The dosage of each

additive complied with manufacturer instructions and previous experimental results as well (6% by RAP

bitumen weight for both additives A and B and 3% by total bitumen weight for additive C).

All the bitumens investigated in this study are coded and summarised in Table 3.

5 Experimental program and test procedure

As bitumen is a viscoelastic material, it exhibits both elastic and viscous components of response and its

stress-strain relationship is both temperature- and time- dependent. Bitumen rheology is consequently

7
defined by its strain-stress-time-temperature response. However, within the linear viscoelastic (LVE)

region, the interrelation between strain and stress is influenced by temperature and time alone and not

by the strain magnitude (Van der Poel, 1954).

Table 3 Investigated bitumens.

Bitumen type
Bitumen preparation
Code Name

VB Virgin bitumen The reference bitumen 50/70

Bitumen 50/70 subjected to a short-term ageing by

STAG Short-term aged bitumen
means of RTFOT
Long-term aged Bitumen 50/70 subjected to a long-term ageing by means
LTAG
bitumen/RAP bitumen of RTFOT + PAV
RAP bitumen blended with virgin bitumen 50/70 in
LTAG+VB Unrejuvenated bitumen
proportion 50/50
RAP bitumen blended with 6% of rejuvenator A and virgin
LTAG+VB+A Rejuvenated bitumen type A
bitumen 50/70 in proportion 50/50
RAP bitumen blended with 6% of rejuvenator B and virgin
LTAG+VB+B Rejuvenated bitumen type B
bitumen 50/70 in proportion 50/50
RAP bitumen blended with virgin bitumen 50/70 in
LTAG+VB+C Rejuvenated bitumen type C
proportion 50/50 and 3% of rejuvenator C
Short-term aged Unrejuvenated bitumen subjected to a short-term ageing
LTAG+VB_STAG
unrejuvenated bitumen by means of RTFOT
Short-term aged rejuvenated Rejuvenated bitumen type A subjected to a short-term
LTAG+VB+A_STAG
bitumen type A ageing by means of RTFOT
Short-term aged rejuvenated Rejuvenated bitumen type B subjected to a short-term
LTAG+VB+B_STAG
bitumen type B ageing by means of RTFOT
Short-term aged rejuvenated Rejuvenated bitumen type C subjected to a short-term
LTAG+VB+C_STAG
bitumen type C ageing by means of RTFOT
Long-term aged Unrejuvenated bitumen subjected to a long-term ageing
LTAG+VB_LTAG
unrejuvenated bitumen by means of RTFOT + PAV
Long-term aged rejuvenated Rejuvenated bitumen type A subjected to a long-term
LTAG+VB+A_LTAG
bitumen type A ageing by means of RTFOT + PAV
Long-term aged rejuvenated Rejuvenated bitumen type B subjected to a long-term
LTAG+VB+B_LTAG
bitumen type B ageing by means of RTFOT + PAV
Long-term aged rejuvenated Rejuvenated bitumen type C subjected to a long-term
LTAG+VB+C_LTAG
bitumen type C ageing by means of RTFOT + PAV

Based on the above-mentioned bitumen properties, a rheological characterisation of each bitumen

selected was carried out by running tests, under different conditions, which allowed two main

parameters to be determined: the LVE strain limit (γlim) and the complex modulus (G*). Strain sweep

tests were performed in order to determine the LVE region of the bitumens, i.e., where the norm of the

complex modulus |G*| is not influenced by the strain magnitude. In particular, bitumen response was

8
studied at a constant frequency (f = 1.59 Hz) by applying a range of strains (γ = 0.003-3%) for each

temperature selected (T = 4, 16 and 28 ℃), in order to monitor |G*| and thus determine the threshold of

LVE region, γlim (defined as the strain corresponding to a |G*| deviation equal to 5% referred to its initial

value |G*in|). Frequency sweep tests conducted under different temperatures and loading conditions

represent a useful tool for a complete characterisation of bitumen viscoelastic properties. In addition,

these tests implemented for thermo-rheologically simple bitumens at a strain within LVE region (i.e., γ <

γlim) enable experimental data to be shifted between different frequencies and temperatures by applying

the time-temperature superposition principle (TTSP). In particular, frequency sweep tests were carried

out at a constant strain (γ = 0.5% < γlim) over a range of frequencies (from 0.159 to 15.9 Hz) and

temperatures (from 4 to 82 ℃, with 6 ℃ intervals).

A dynamic shear rheometer (DSR) was used for both strain and frequency sweep tests. The tests

were set up in plate-plate configuration (diameter of 8 mm and gap of 2 mm for low and intermediate

temperatures; diameter of 25 mm and gap of 1 mm for high temperatures) and the sinusoidal load was

applied in control-strain mode. In accordance with EN 14770, the test protocol provided 2 repetitions for

each test. In case of result dispersion (|G*| out of the range of 10%), a third repetition was carried out.

6 Analysis and discussion of the results

6.1 Identification of LVE region

Before running the frequency sweep tests, strain sweep tests were carried out on the long-term aged

unrejuvenated bitumen (LTAG+VB_LTAG), which exhibits the worst condition in terms of brittleness, as

a consequence of hardening due to ageing effects. In fact, the more severe the oxidation subjected by

the bitumen considered, the higher the |G*| values measured and the lower γlim (Grilli et al., 2017).

Results summarised in Table 4 and depicted in Fig. 1 allow the threshold of LVE region, γlim, to be

identified and consequently a proper strain value within LVE region to be selected for frequency sweep

test implementation.

9
 Table 4 Strain sweep test data for the long-term aged unrejuvenated bitumen.

Temperature
Bitumen Repetition
28 ℃ 16 ℃ 4℃

N. |G*| [Pa] lim (%) |G*| (Pa) lim [%] lim (%) |G*| (Pa)

LTAG+VB_LTAG 1 1.21E+07 1.53 3.33E+07 1.44 7.85E+07 1.40

2 1.21E+07 1.68 3.35E+07 1.51 7.84E+07 1.47

Fig. 1 Strain sweep test isotherms for the long-term aged unrejuvenated bitumen

6.2 Data analysis and modelling

Before the construction of the master curves, Black and Cole-Cole diagrams were plotted as useful

representations of raw data obtained from frequency sweep tests for all the bitumens investigated. The

Black diagram is the graph of the norm of the complex modulus |G*| versus the phase angle δ. A smooth

curve in Black diagram is a useful indicator of time-temperature equivalency and thermo-rheologically

simplicity for the bitumens tested (Lesueur et al, 1996) as well as no discrepancies in experimental

results (Airey, 2002); moreover, through this plot the magnitude of the glassy asymptote can be

reasonably estimated and used in the master curve construction. The Cole-Cole diagram is the graph of

the loss modulus, G2 as a function of the storage modulus G1; it allows immediately appreciating the

ratio between the two complex modulus components and thus estimating the preponderance of the

viscous or elastic behaviour at the different temperatures investigated.

As resulted in the Black Diagrams depicted in the following sections of the current paragraph (Figs.

3a-6a), all the bitumens studied can be considered as linear viscoelastic under the conditions

considered and characterised as thermo-rheologically simple, thus TTSP was applied to generate

10
complex modulus master curves and shift factor relationship. A reference temperature equal to 34 ℃

was selected and the rheological data at all the other temperatures were shifted with respect to time until

the curves merge into a single smooth function. The modified Christensen-Anderson-Marasteanu

(CAM) Model was adopted to relate the complex modulus norm to the reduced frequency, following a

shift factor variation based on the Williams-Landel-Ferry (WLF) law. In detail, according to the modified

CAM model, the equation for complex modulus norm is given by Eq. (1)

Gg*  Ge*
G G 
* *
e me
Errore. L'origine riferimento non è stata trovata.
  f   k k

1   c'  
  f  

(1)

where Ge*  G* ( f  0) is the equilibrium complex modulus ( Ge*  0 for bitumens while Ge*  0 for

mixtures in shear), Gg*  G* ( f  ) is the glass complex modulus, fc is the location parameter with

dimension of frequency (i.e., crossover frequency), f’ is the reduced frequency (function of both

temperature and strain), k and me are dimensionless shape parameters.

Fig. 2 Model for complex modulus master curve (Bahia et al., 2001).

Fig. 2 illustrates the complex modulus master curve in Eq. (1). It can be seen that Gg* is the horizontal

asymptote at f→∞, and Ge* is the horizontal asymptote at f→0. The Ge* asymptote is zero for

bitumens. The third asymptote is the one with a slope of me and represents the viscous asymptote. The

Gg* and me asymptotes intercept at fc, whereas the intercept between Ge* and me asymptotes is defined

by Eq. (2)

11
 1
 G*  me
f c'  f c  e*  Errore. L'origine riferimento non è stata trovata.
 Gg 
 
(2)

where f c' = 0 for bitumens.

The distance between G* ( fc' ) and Gg* for bitumens is given by Eq. (3)

me
2k
R  Log Errore. L'origine riferimento non è stata trovata.
 mke  Ge*
1   2  1 *
  Gg
(3)

where Gg* = 0, thus R = me/k Log2 for bitumens.

The distance between G* ( fc' ) and Ge* for bitumens is given by

  me

  G*   k

 Gg  e  
k
* m
 
R  Log 1   *  1 1   *    Errore. L'origine riferimento non è stata trovata.
' g
   
  Ge    Ge   
   


(4)

where Gg* = 0, thus R’ = Log2 for bitumens.

The WLF formulation is then used in the modified CAM model to express the temperature-shift factor

aT T  C T  T0 
log  1 Errore. L'origine riferimento non è stata trovata.
aT T0  C2  T  T0 

(5)

where aT is the shift factor at temperature T, T0 is the reference temperature, C1 and C2 are constants.

6.3 Effects of ageing on virgin bitumen

All the curves plotted in Fig. 3 and data summarised in Table 5 clearly show an increase in |G*| values,

12
indicating a marked bitumen hardening, and a reduction in phase angles δ. Hence, the results indicate a

prevalence of the elastic component G1 on the viscous component G2, as a consequence of the ageing

subjected by the reference virgin bitumen. Moreover, considering the CAM model parameters

summarised in Table 6, oxidation phenomena determine the following effects on the reference bitumen:

- lower shape index S, as an evidence of a higher sensitivity to frequency changes;

- lower crossover frequency fc, suggesting a greater overall elastic component in the behaviour;

- higher C1 and C2 values, according to the reduction in fractional free volume (i.e., reduction of

molecular mobility) (Mazzoni et al., 2016). Discussion part should explore the significance of the results

of the work, not repeat them. A combined results and discussion section is often appropriate. Avoid

extensive citations and discussion of published literature.

Table 5 Rheological data obtained for the reference bitumen investigated at different stages of ageing (virgin, short- and long-term aged
bitumen) for f = 1.59 Hz.

T=4℃ T = 58 ℃
Bitumen
|G*| (Pa) G1 (Pa) G2 (Pa) δ (°) |G*| (Pa) G1 (Pa) G2 (Pa) δ (°)

VB 2.09E+07 1.49E+07 1.46E+07 44.3 3.60E+03 2.58E+02 3.59E+03 85.9

STAG 3.74E+07 3.12E+07 2.06E+07 33.5 1.63E+04 3.03E+03 1.61E+04 79.3

LTAG 6.79E+07 6.18E+07 2.81E+07 24.4 1.19E+05 4.97E+04 1.08E+05 65.1

Table 6 Calibrated parameters of the modified CAM model and WLF law for the reference bitumen investigated at different stages of
ageing (virgin, short- and long-term aged bitumen).

Gg  Ge
* *

G  Ge 
* *
C1 (T  Ta )
fc
mc
log( a1 ) 
[1  (
k
) ]k C2  (T  Ta )
CAM
f
modified mg
model + k
WLF law 2
* * S  log
Ge Gg fc
k me
mg * 2
C1 C2 T0 (℃)
(Hz) Ge R
(Pa) (Pa) 1  (2 k
 1) *
Gg

VB 0 1E+09 360 0.16 1.12 2.107 0.996 15 168 34

STAG 0 1E+09 290 0.16 0.96 1.797 0.995 21 210 34
LTAG 0 1E+09 280 0.14 0.70 1.479 0.987 26 210 34

13
(a) (b)

(c)

Fig. 3 Rheological characterisation of the reference bitumen investigated at different stages of ageing (virgin, short- and long-term aged
bitumen). (a) Black diagram. (b) Cole-Cole diagram. (c) Master curves of |G*| at 34 ℃.

6.4 Effects of bitumen rejuvenation

Rejuvenators modify bitumen chemistry and, consequently, rheology by enhancing the viscous

response of the bitumen (Nahar et al., 2014, Xu et al., 2014). This behaviour results in a decrease in |G*|

values, indicating a bitumen softening, and a rise of phase angles δ, corresponding to a lower G1/G2 ratio,

as shown in Fig. 4 and Table 7, comparing the rejuvenated bitumens to the associated composite

bitumen without additive (LTAG+VB+A/B/C versus LTAG+VB). In addition, with respect to the CAM

model parameters summarised in Table 8, the presence of each rejuvenator leads to the following

effects on the corresponding composite bituminous blend (LTAG+VB+A/B/C versus LTAG+VB):

14
 - higher shape index S, as an indication of a more gradual transition from the elastic to the viscous

behaviour;

- higher crossover frequency fc, and thus a remarkable retrieval of viscous component in the

behaviour;

- lower C1 and C2 values, as a consequence of higher molecule mobility.

On the overall, the additives used are even approaching to restore the rheological properties of the

virgin bitumen contained in each composite bituminous blend where they are implemented

(LTAG+VB+A/B/C versus VB). This result is confirmed by the comparable values of the calibrated

parameters summarised in Table 8 and the nearing of the rheological data and curves shown in Table 7

and Fig. 4 (LTAG+VB+A/B/C versus VB).

Table 7 Rheological data obtained for the unrejuvenated bitumen and the rejuvenated bitumens with associated virgin and long-term aged
bitumens at f = 1.59 Hz.

T=4℃ T = 58 ℃
Bitumen
|G*| (Pa) G1 (Pa) G2 (Pa) δ (°) |G*| (Pa) G1 (Pa) G2 (Pa) δ (°)

VB 2.09E+07 1.49E+07 1.46E+07 44.3 3.60E+03 2.58E+02 3.59E+03 85.9

LTAG+VB+A 1.98E+07 1.59E+07 1.19E+07 36.8 7.45E+03 1.04E+03 7.39E+03 82.0
LTAG+VB+B 2.66E+07 2.11E+07 1.62E+07 37.6 7.62E+03 9.48E+02 7.56E+03 82.9
LTAG+VB+C 2.20E+07 1.77E+07 1.30E+07 36.4 1.08E+04 1.71E+03 1.07E+04 80.9
LTAG+VB 4.47E+07 3.84E+07 2.30E+07 31.0 1.64E+04 3.09E+03 1.61E+04 79.1
LTAG 6.79E+07 6.18E+07 2.81E+07 24.4 1.19E+05 4.97E+04 1.08E+05 65.1

Table 8 Calibrated parameters of the modified CAM model and WLF law for the unrejuvenated bitumen and the rejuvenated bitumens with
associated virgin and long-term aged bitumens.

Gg  Ge
* *

G  Ge 
* *
C1 (T  Ta )
fc
mc
log( a1 ) 
[1  (
k
) ]k C2  (T  Ta )
CAM f
modified
mg
model +
WLF law k
2
S  log
* *
Ge Gg fc
k me mg 2
C1 C2 T0 (℃)
* R
(Pa) (Hz) Ge
(Pa) 1  (2 k
 1) *
Gg
VB 0 1E+09 360 0.16 1.12 2.107 0.996 15.0 168 34

15
LTAG+VB+A 0 1E+09 360 0.16 1.06 1.994 0.993 18.5 190 34
LTAG+VB+B 0 1E+09 400 0.16 1.03 1.938 0.994 17.0 180 34
LTAG+VB+C 0 1E+09 400 0.16 1.01 1.900 0.991 15.5 165 34
LTAG+VB 0 1E+09 380 0.16 0.92 1.731 0.969 22.5 200 34
LTAG 0 1E+09 280 0.14 0.70 1.479 0.987 26.0 210 34

(a) (b)

(c)

Fig. 4 Comparison among the unrejuvenated bitumen and the rejuvenated bitumens with the associated virgin and long-term aged bitumens. (a)
Black diagram. (b) Cole-cole diagram. (c) Master curves of |G*| at 34 ℃.

6.5 Effects of ageing on hot recycled bituminous blends

The results from the bituminous blends including 50% of RAP bitumen and 50% of virgin bitumen, with

or without rejuvenator (LTAG+VB and LTAG+VB+A/B/C versus LTAG+VB_LTAG and

LTAG+VB+A/B/C_LTAG), are shown in Tables 9 and 10 and the corresponding master curves, at

different ageing levels, are plotted in Fig. 5. For these binders, the oxidation causes the same

above-mentioned effects as for the reference virgin bitumen (Fig. 3 and Tables 4 and 5). However, since

16
the hot recycled bitumen blends (rejuvenated or not) are composed of 50% RAP bitumen, oxidation is

less detrimental on them than on the virgin bitumen, as confirmed by a lower variation of parameter

values with ageing. Moreover, it should be highlighted that the addition of a rejuvenator in hot recycling

leads to a composite bituminous blend which can be even less stiff (lower |G*| values) than the

associated virgin bitumen alone at the end of service life, suggesting significant benefits when dealing

with high RAP contents (Fig. 6) (LTAG+VB+A/B/C_LTAG versus LTAG). In detail, with respect to the

associated reference bitumen alone, the rejuvenated bitumens type B or A guarantee lower ageing

effects for T < 58 ℃ and a comparable or slightly higher hardening for T ≥ 58 ℃, respectively (Fig. 7)

(LTAG+VB+B/A_LTAG versus LTAG). Whereas the long-term aged rejuvenated bitumen type C

exhibits similar stiffness values at temperatures lower than 58 °C and a doubling in stiffness values at

higher temperatures (T ≥ 58 ℃ ), if compared to the associated reference bitumen alone (Fig. 7)

(LTAG+VB+C_LTAG versus LTAG).

In particular, with respect to the associated reference bitumen alone, the additive A provides a lower

consistency to the corresponding rejuvenated bitumen also when it is unaged or short-term aged,

especially at T < 58 ℃ , as shown by the rheological data in Tables 9 and 5 (LTAG+VB+A and

LTAG+VB+A_STAG versus VB and STAG). Whereas the presence of additives B in the bituminous

blends allows obtaining optimum performance during all the service life, as confirmed by the positive

rheological values in Table 9 compared to those from the associated reference bitumen in Table 5

(LTAG+VB+B pre- and post-ageing versus VB/LTAG). This positive behaviour results in a slightly higher

stiffness for this rejuvenated bitumen when it is unaged or short-term aged (LTAG+VB+B,

LTAG+VB+B_STAG), and lower stiffness after long-term ageing process (LTAG+VB+B_LTAG),

suggesting a likely higher resistance to rutting, fatigue and thermal cracking, respectively. As concerns

the rejuvenated bitumen type C, its mechanical response is quite comparable to that of the associated

reference bitumen alone at the different stages of ageing, except for T ≥ 58 ℃ when doubled stiffness

values occur, as suggested by the rheological data in Tables 9 and 5 (LTAG+VB+C pre and post ageing

versus VB/LTAG).

17
Table 9 Rheological data obtained for the hot recycled bitumens (rejuvenated or not) at f = 1.59 Hz investigated at different ageing stages.

T=4℃ T = 58 ℃
Bitumen
|G*| (Pa) G1 (Pa) G2 (Pa) δ (°) |G*| (Pa) G1 (Pa) G2 (Pa) δ (°)

LTAG+VB 4.47E+07 3.84E+07 2.30E+07 31.0 1.64E+04 3.09E+03 1.61E+04 79.1

LTAG+VB_STAG 5.88E+07 5.28E+07 2.59E+07 26.2 8.75E+04 3.45E+04 8.04E+04 66.8
LTAG+VB_LTAG 8.36E+07 7.78E+07 3.05E+07 21.4 3.47E+05 2.01E+05 2.83E+05 54.6
LTAG+VB+A 1.98E+07 1.59E+07 1.19E+07 36.8 7.45E+03 1.04E+03 7.39E+03 82.0
LTAG+VB+A_STAG 3.25E+07 2.77E+07 1.70E+07 31.5 3.38E+04 1.05E+04 3.21E+04 71.9
LTAG+VB+A_LTAG 5.39E+07 4.91E+07 2.23E+07 24.5 1.42E+05 7.10E+04 1.23E+05 60.0
LTAG+VB+B 2.66E+07 2.11E+07 1.62E+07 37.6 7.62E+03 9.48E+02 7.56E+03 82.9
LTAG+VB+B_STAG 4.01E+07 3.46E+07 2.02E+07 30.2 3.13E+04 8.84E+03 3.00E+04 73.6
LTAG+VB+B_LTAG 5.90E+07 5.36E+07 2.45E+07 24.6 1.14E+05 5.04E+04 1.02E+05 63.7
LTAG+VB+C 2.20E+07 1.77E+07 1.30E+07 36.4 1.08E+04 1.71E+03 1.07E+04 80.9
LTAG+VB+C_STAG 3.87E+07 3.32E+07 1.99E+07 30.9 3.13E+04 8.78E+03 3.00E+04 73.7
LTAG+VB+C_LTAG 6.57E+07 6.02E +07 2.64E +07 23.7 1.99E+05 1.02E+05 1.71E+05 59.2

(a) (b)

(c) (d)

18
 Fig. 5 Master curves of |G*| at 34 ℃ for the hot recycled bitumens (rejuvenated or not) investigated at different ageing stages.

Table 10 Calibrated parameters of the modified CAM model and WLF law for the hot recycled bitumens (rejuvenated or not) investigated at
different ageing stages.

Gg  Ge
* *

G  Ge 
* *
C1 (T  Ta )
fc
mc
log( a1 ) 
[1  (
k
) ] k
C2  (T  Ta )
f
CAM modified
mg
model +
WLF law k
2
* * fc S  log
Ge Gg k me
mg * 2
C1 C2 T0 (℃)
(Hz Ge R
(Pa) (Pa) ) 1  (2 k
 1) *
Gg

LTAG+VB 0 1E+09 380 0.16 0.90 1.693 0.970 19.5 175 34

LTAG+VB_STAG 0 1E+09 260 0.15 0.78 1.565 0.982 22.0 185 34
LTAG+VB_LTAG 0 1E+09 225 0.15 0.65 1.339 0.983 27.0 215 34
LTAG+VB+A 0 1E+09 360 0.16 1.06 1.994 0.993 18.5 190 34
LTAG+VB+A_STAG 0 1E+09 350 0.16 0.89 1.728 0.990 22.0 220 34
LTAG+VB+A_LTAG 0 1E+09 240 0.16 0.75 1.457 0.988 27.5 240 34
LTAG+VB+B 0 1E+09 400 0.16 1.03 1.938 0.994 17.0 180 34
LTAG+VB+B_STAG 0 1E+09 340 0.15 0.86 1.726 0.990 22.0 200 34
LTAG+VB+B_LTAG 0 1E+09 260 0.15 0.75 1.495 0.988 27.5 230 34
LTAG+VB+C 0 1E+09 400 0.16 1.01 1.900 0.991 15.5 165 34
LTAG+VB+C_STAG 0 1E+09 340 0.15 0.86 1.726 0.992 21.5 200 34
LTAG+VB+C_LTAG 0 1E+09 250 0.17 0.73 1.332 0.990 24.0 220 34

(a) (b)

19
(c)

Fig. 6 Comparison among all the long-term aged bitumens. (a) Black diagram. (b) Cole-cole diagram. (c) Master curves of |G*| at 34 ℃.

(a)

(b)

20
(c)

Fig. 7 Comparison among the long-term aged bitumens investigated in terms of |G*| at f=1.59 Hz.

7 Conclusions

The experimental investigation described in this paper focused on the assessment of the rheological

properties of a reference bitumen considered during its overall service life that includes its reuse in hot

recycling by adopting different rejuvenators.

Based on the results obtained, the following conclusions can be drawn:

- Ageing entails an increase in |G*| values, indicating a bitumen hardening, and a reduction in

phase angles δ, corresponding to a prevalence of the elastic component G1 over the viscous component

G2. In addition, the analysis of the master curve parameters shows a decrease in shape index S, as an

evidence of a higher sensitivity to frequency changes, and in crossover frequency fc, suggesting a

greater overall elastic behaviour. Moreover, higher C1 and C2 values are a further consequence of

oxidation according to the reduction in fractional free volume (i.e., reduction of molecular mobility).

- Rejuvenators modify bitumen chemistry and consequentl rheology by enhancing the viscous

response of the bitumen, as confirmed by a decrease in |G*| values and a rise of phase angles δ,

corresponding to a lower G1/G2 ratio. In terms of master curve parameters, compared to the

corresponding unrejuvenated bitumen, bitumens including any rejuvenator exhibit higher shape index S,

as an indication of a more gradual transition from the elastic to the viscous behaviour, and crossover

frequency fc, and thus a remarkable retrieval of viscous component in the behaviour. Moreover, all the

additives used are even approaching to restore the rheological properties of the virgin bitumen, because

21
of the comparable values obtained for both model and rheological parameters.

- Ageing has a similar effect on virgin bitumen and bituminous blends including RAP bitumen.

However, as confirmed by a lower variation of parameter values pre and post ageing, oxidation is less

detrimental on the hot recycled bitumens (rejuvenated or not) than on the virgin bitumen, since the

former are composed of 50% of aged RAP bitumen.

- The addition of a rejuvenator in hot recycling leads to a corresponding composite bituminous

blend which can be even less stiff than the associated virgin bitumen alone at the end of service life,

suggesting significant benefits when dealing with high RAP contents. In particular, if compared to the

associated virgin bitumen alone, the rejuvenated bitumens type B and A guarantee lower ageing effects

in a wide range of temperatures (up to 58 ℃), whereas in the same range of temperatures the

rejuvenated bitumen type C exhibits similar stiffness values pre and post ageing. At higher temperatures

(T ≥ 58 ℃) a comparable, slightly higher or even doubled hardening occur, when the additive B, A or C

is selected as rejuvenator, respectively.

In conclusion, this experimental study provides an important contribution to understand the effect of

ageing on the rheological properties of the bituminous blends containing virgin and RAP bitumens.

Based on the above-described findings, it is reasonable to expect that recycled asphalt mixtures

prepared with virgin bitumens, rejuvenators and high amounts of RAP (which releases a percentage of

the same aged bitumen) suffer less ageing phenomena and could also be less stiff than virgin mixtures.

However, great importance should be given to the choice of the most suitable components of the

mixture due to compatibility. In particular, type and dosage of rejuvenator should be properly selected,

since their interaction strongly affects the final mixture performance. In addition, it is likely expected that

using the same rejuvenators with a different base bitumen could change the corresponding bitumen

response. Therefore, further analyses on different types of base bitumens are in progress for a better

understanding of their influence on rejuvenation.

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26
Giorgia Mazzoni is a Ph. D from the Università Politecnica delle Marche (Italy). She is mainly involved

in the evaluation of the effects linked to hot recycling of high RAP contents on the binder performance. In

particular, her research area focused on classic and advanced rheological characterisation of bitumens

and bituminous mastic in terms of fatigue, thixotropy and self-healing.

Edoardo Bocci is Assistant Professor at eCampus University (Italy). His research field deals with

paving materials for steel deck bridges, recycling of reclaimed asphalt through hot and cold techniques,

reuse of wastes in bituminous mixtures (C&D, fibers and crumb rubber from end-of-life tires, steel

slags), rheological characterization of materials for road pavements, evolution of damage in asphalt

mixtures.

27
 Francesco Canestrari is Full Professor of Roads, Railways and Airports and Chair of the Master

degree in Civil Engineering at the Università Politecnica delle Marche (Italy).

Professor Canestrari is involved as principal investigator in several international research projects. His

specialty areas include testing specifications, interface shear characterisation of asphalt layers,

reinforced pavements, rheological and performance based characterisation of sustainable and

innovative pavement materials.

28

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