Construction and Building Materials 67 (2014) 270–278

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Construction and Building Materials

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

Toward more realistic viscosity measurements of tyre rubber–bitumen

blends
Davide Lo Presti a,⇑, Claudia Fecarotti a, Adam T. Clare b, Gordon Airey a
a
Nottingham Transportation Engineering Centre, University of Nottingham, Nottingham, UK
b
Precision Manufacturing Centre, University of Nottingham, Nottingham, UK

h i g h l i g h t s g r a p h i c a l a b s t r a c t

 Introducing the practical issue with

viscosity measurements of recycled
tyre rubber modified bitumen.
 Rapid prototyping and visual
assessment and dual helical impeller
manufacturing.
 Dual helical impeller calibration.
 Validation of results through
comparison with viscosity
measurements undertaken with a
standard impeller.
 Adapting the rotational viscometer as
a low-shear mixer by using the DHI.

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

Article history: The measurement of rheological properties of the tyre rubber bitumen blends is often challenging due to
Received 14 August 2013 presence of suspended tyre rubber’s crumbs. Furthermore, the phase separation during the course of
Received in revised form 24 March 2014 measurements makes the viscosity of these non-homogeneous blends difficult to ascertain. In this study,
Accepted 25 March 2014
a new dual helical impeller was designed and manufactured to be used with a rotational viscometer in
Available online 13 April 2014
order to have a real-time control of the viscosity while performing a laboratory mixing of the blends.
Layer based manufacturing techniques showed to be a convenient method to produce complex shaped
Keywords:
impeller prototypes before manufacturing the more expensive stainless steel assembly. Impeller geom-
Dual helical impeller
Rapid prototyping
etry was optimised to create a convective like flow within the sample and so minimise phase separation.
Electrical discharge machining Shear rate constant is geometry dependent and a calibration exercise was carried out to ascertain this.
Viscometry Results of both calibration and validation phases showed that the new impeller provides reliable viscosity
Recycled tyre rubber measurements of homogenous fluids such as neat bitumen. With regards to complex fluids the new
Rubberised bitumen impeller showed a more stable and realistic trend than that obtained by using a standard spindle. In fact,
it was demonstrated that the new impeller significantly decreases phase separation within the blend and
in turns provides a more realistic measurement of the viscosity. This system represents a feasible and
improved solution for optimising the laboratory modification process of tyre rubber bitumen blends
by adapting the rotational viscometer as a low-shear mixer.
Ó 2014 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND
license (http://creativecommons.org/licenses/by-nc-nd/3.0/).

Abbreviations: EDM, electrical discharge machining; ELTs, end-of-life tyres; FDM, fused deposition modelling; HA, high torque viscometer; LV, low torque viscometer;
RTR-MB, recycled tyre rubber modified bitumen; RTR, recycled tyre rubber; SRC, shear rate constant.
⇑ Corresponding author. Tel.: +44 7587140422.
E-mail addresses: davide.lopresti@nottingham.ac.uk (D. Lo Presti), evxcf@nottingham.ac.uk (C. Fecarotti), adam.clare@nottingham.ac.uk (A.T. Clare), gordon.airey@
nottingham.ac.uk (G. Airey).

http://dx.doi.org/10.1016/j.conbuildmat.2014.03.038
0950-0618/Ó 2014 The Authors. Published by Elsevier Ltd.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/3.0/).
 D. Lo Presti et al. / Construction and Building Materials 67 (2014) 270–278 271

1. Introduction the polymeric chains that are the main components of the rubber,
both natural and synthetic, contained in the RTR. The absorption of
1.1. Background aromatic oils from the bitumen into the rubber’s polymer chains
causes the rubber to swell and soften [17]. RTR particles are swol-
The accumulation of end-of-life tyres (ELTs) and premature len by the absorption of the bitumen oily phase at high tempera-
pavement failures are both interconnected and dependant of each tures (160–220 °C) into the polymer chains, which are the key
other due to enormous increase in traffic density and axle loading components of the RTR-MB to form a gel-like material. Therefore,
respectively. The use of RTR in asphalt pavements started 170 years during the reaction there is a contemporaneous reduction in the
ago, with an experiment involving natural rubber with bitumen in oily fraction and an increase of rubber particle sizes with a conse-
the 1840s [1], attempting to capture the flexible nature of rubber in quent reduction of the inter-particle distance. This implies the for-
a longer lasting paving surface. In 1960s scrap tyres were processed mation of gel structures that produce a viscosity increase up to a
and used as a secondary material in the pavement industry. One factor of 10 [1].
application was introduced by Charles McDonald, a materials engi- Rubber reacts in a time–temperature dependent manner
neer of the city of Phoenix in Arizona (USA), who was the first to (Fig. 2). If the temperature is too high or the time is too long, the
find that after thoroughly mixing crumbs of RTR with bitumen swelling will continue to the point where, due to long exposure
and allowing it to react for a period of forty-five minutes to an hour, to the high temperatures, swelling is replaced by depolymerisa-
this material captured beneficial engineering characteristics of both tion/devulcanisation which causes dispersion of the rubber into
base ingredients. He called it Asphalt Rubber and the technology is the bitumen. Depolymerisation starts releasing rubber compo-
well known as the ‘‘Wet process’’. By 1975, crumb rubber was suc- nents back to the liquid phase causing a decrease in the stiffness
cessfully incorporated into asphalt mixtures and in 1988 a defini- (G*) while the elastic properties (d) continues to modify (Fig. 1a
tion for rubberised bitumen was included in the American Society and b). If temperature is high or time is long enough, depolymer-
for Testing and Materials (ASTM) D8 and later specified in ASTM isation will continue causing more destruction of the binder net-
D6114-97. In 1992 the patent of the McDonald’s process expired working and so d modification is lost [18]. The interaction
and the material is now considered a part of the public domain. Fur- between bitumen and rubber materials is material-specific and
thermore, in 1991, the United States federal law named ‘‘Inter- RTR-MBs are extremely dependent on the variability of these pro-
modal Surface Transportation Efficiency Act’’ (then rescinded), cessing conditions, particularly to what concerns the temperature
mandated its widespread use, the Asphalt–Rubber technology con- and time of reaction [19–21]. RTR-MBs must be properly designed
cept started to make a ‘‘quiet come back’’ [2]. and, where necessary, produced to comply with specifications and
Nowadays, these rubberised bitumen materials, obtained provide a quality product suitable for the expected climate and
through the wet process, have spread worldwide as solutions for traffic conditions. Research is still on-going worldwide to validate
different quality problems (asphalt binders, pavements, stress and improve technologies related to rubberised bitumens and
absorbing lays and inlayers, roofing materials, etc.) with much dif- particularly to what concern the monitoring of the quality of the
ferent evidence of success demonstrated by roads built in the last rubber–bitumen blends in the field-production as well as in the
30 years. Since the invention of McDonald, the wet process tech- laboratory design stage. A key property of RTR-MBs that needs par-
nology has been used and modified more widely in four states in ticular attention and definitely further improvement in its evalua-
the US: Arizona, California, Texas, and Florida. More recently wet tion is viscosity. In fact as a consequence of the non-homogeneity
process has been used also in South Carolina, Nevada and New of this material, ASTM D-6114 specification uses the concept of
Mexico. South Africa and Australia started introducing bitumen– ‘‘apparent viscosity’’ to categorise the different type of rubberised
rubber as a binder for asphalt and for seals from the early 1980s binders. This means that as opposed to more homogeneous mate-
and mid 1970s respectively [3,4]. In Europe wet rubberised asphalt rials (i.e. neat bitumen) to evaluate the viscosity of RTR-MBs prop-
has been successfully used in road pavements application since erly, information must be given about the shear conditions [22]. In
1981 in Belgium, as well as in France, Austria, Netherlands, Poland this sense ASTM D6114 specifies to use rotational viscometer in
and Germany [5], more recently also in Greece [6] and UK [7], but low shear by performing measurements at 12 or 20 rpm depending
the countries with a higher numbers of applications are Portugal on the type of viscometer: low torque (LV model), or high torque
[8], Spain [9], Italy [10], Czech Republic [11] and Sweden [12]. (HA model).
Nowadays the rubberised asphalt technology is being adopted in Since viscosity is the key properties monitored during the field-
many other parts of the world: Taiwan was reported to have production and laboratory design of bitumen–rubber blend [24], in
adopted wet process rubberised asphalt mixtures for flexible pave- a previous study [25] a rotational viscometer has been adapted to
ment rehabilitation [4]; furthermore, wet process rubberised act as a low shear mixer able to provide real-time viscosity mea-
asphalt has been trialled in Beijing and for use in new and mainte- surements. This solution helps optimising a RTR–bitumen blend
nance work as part of the preparation for the 2008 Olympics in with an accurate control of temperature and by consuming only
China and it has also been used in EcoPark Project in Hong Kong. a small amount of the materials. Nevertheless, this procedure pre-
On the basis of first positive experiences also Brazil [13] and Sudan sents some downside due to phase separation occurring during the
[14] are strongly investing in the application of this technology for mixing process. In fact RTR particles tend to float on the surface,
road pavements. thus a manual movement up and down of a standard impeller is
The term ‘‘wet process’’ refers to a whole family of technologies necessary to keep a good distribution of the particles within the
which varies a lot with regards with the chosen processing condi- blend. Of course, this practice affects the viscosity measurements
tions. The nature of the mechanism by which the interaction be- and could damage the equipment. The rotational viscometer used
tween bitumen and RTR crumbs takes place has not been fully in this previous study (commonly used worldwide) can be
characterised. Traditionally it is reported that bitumen–rubber equipped with special accessories and impellers that can help with
interaction is not chemical in nature [1], but other studies claim the measure of viscosity of the blend with suspended particles
that the increase in binder viscosity cannot be accounted for only [26]. Nevertheless, none of them is apparently able to provide a
by existence of the rubber swelling particles [16]. The reaction it- better distribution of the particles through the sample volume.
self is made up of two simultaneous processes (Fig. 1): partial Therefore, when dealing with complex materials, such as RTR-
digestion of the rubber into the bitumen on one hand and, on the MBs, there is the need of some innovation to improve standard
other, adsorption of the aromatic oils available in this latter within rotational viscometers to adapt them as a low-shear mixer for
272 D. Lo Presti et al. / Construction and Building Materials 67 (2014) 270–278

Fig. 1. Bitumen–RTR interaction phenomenon at elevated temperatures: change of properties over time. Adapted from [15].

viscometer. The idea of this type of impeller has been investigated

within research conducted in other fields [27,28] but the adapta-
tion to the tyre rubber–bitumen blending process and the actual
manufacturing and calibration of a stainless steel impeller for the
specific equipment is an original work of this research. The study
has been developed in two phases: a preliminary study, involving
the rapid prototyping of the helical impeller and a visual control
of its validity; secondly the manufacture of a stainless steel impel-
ler followed by its calibration and validation to obtain more realis-
tic viscosity measurements.

2. Dual helical impeller manufacture

Fig. 2. Typical changes in viscosity values from RTR-MBs at different temperatures
over time. Adapted from [23].
2.1. Rapid prototyping

laboratory design of the blends and to improve the meaningfulness In order to understand the effect of the dual helical impeller
of the viscosity measurements. (DHI) a preliminary study was performed by designing and manu-
facturing a plastic impeller to be used with a mixture of a transpar-
1.2. Aim of the study ent viscosity standard fluid and a high percentage of a ASTM 40#
RTR. The plastic impeller has been designed with a dual helix in or-
With this study the authors aim to design, calibrate and validate der to obtain a convective like flow within the sample. The manu-
a tool which could help limiting phase separations issues of RTR– facture was undertaken using the fused deposition modelling
bitumen blends, so leading to a better mixing process and more (FDM) technique, which is a rapid prototyping technique capable
realistic viscosity measurements. The new impeller helps to get a of realising nested features and texture in recessed surfaces which
better distribution of the particles within the fluid by creating a may not be realised by subtractive methodologies. Perhaps the
convective like flow during the laboratory measurements (Fig. 3). most salient feature of this technique for prototyping work is the
As a consequence the rotational viscometer could be adapted to nominal cost of complexity. That is to say introducing new features
act as a low shear mixer of rubberised bituminous blends and will or modifying designs has little or no cost implications apart from
provide more realistic real-time viscosity measurements. the time invested at the design stage. In this way designs can be
For these reasons, the authors have carried out the following rapidly modified allowing more iteration for experimental work.
investigation which includes the development, calibration and val- This allowed the mixer to be produced as one component without
idation of an original dual helical impeller (DHI) for a rotational the need for assembly.

Fig. 3. The idea through comparison between the impellers and the generated flows during rotation.
 D. Lo Presti et al. / Construction and Building Materials 67 (2014) 270–278 273

2.2. Preliminary visual assessments 2.3. DHI manufacturing

The preliminary study consisted in a comparison of the distri- Fig. 6 shows the DHI manufacturing process which passed
butions of ASTM 40# tyre rubber particles, within a transparent through an initial 3D design of the tool and then through, FDM ra-
fluid of known viscosity, by using the plastic dual helical impeller pid prototyping and the final manufacture in stainless steel. In fact,
and the Brookfield SC 27 (Fig. 4). A viscosity standard fluid was while FDM is a suitable technique for prototypes the current avail-
chosen with a viscosity of about 100 Pa s at 25 °C (1% accuracy), ability of robust materials compatible with this technique are lim-
which is approximately the viscosity of a bitumen pen 40–60 at ited. Due to the inherent requirement of the deposition
160–180 °C. This represents the usual range of temperature at methodology, the polymers used must exhibit a propensity to flow
which the modification of bitumen with RTR is usually performed. at relatively low temperatures; this in turn limits applicability of
The transparency of the fluid allowed the distribution of the parti- the manufactured product to high temperature tests. In the light
cles within the blend to be monitored while the impeller was oper- of this issue and considering that the final application of the DHI
ating at different speeds: 10 RPM and 100 RPM. The study also should allow to use it to mix bituminous blend at over 150 °C,
involved the use of a standard steel impeller, Brookfield SC series the second impeller was manufactured in stainless steel, similar
no 27, with the same blend and rotation speeds. This allowed a vi- to materials used in commercially available instruments. This sec-
sual comparison of the distribution of the particles within the ond DHI was fabricated using a conventional machining approach.
blend by using the two impellers. The analysis was conducted at Due to the necessity of allowing a tool to engage with the work, the
25 °C by monitoring the blends for 15–20 min. This time repre- impeller could not be fabricated as one component and the design
sents the time used to achieve a sufficient thermal equilibrium was modified to form an assembly of two helices. These were fab-
all over the sample before viscosity measurements. ricated separately using a 4-axis machine tool in aluminium ini-
Fig. 4 shows the begin of the visual assessment at the point tially as a test cut and finally in 316L stainless steel for the final
where rubber particles have been added to the fluid and the mixer. Electrical discharge machining (EDM) was also used to re-
blend has been shake to favour a good distribution of the parti- move the core of the outer helix. This technique was selected to
cles. In a second stage both the impellers have been immersed prevent distortion of the slender blade as a result of machining
in the blend and viscometer was turned on to carry out a visual forces. The cost incurred in producing this impeller is significant
assessment at two different rotation speeds: 10 RPM and with respect to producing the FDM mixer discussed earlier and
100 RPM. Fig. 5 shows the distribution of the particles within hence producing low cost, proof of principal prototypes was a vital
the blend after 15–20 min of rotation. Results show that at stage in this study.
10 RPM both standard and DHI do not maintain particles in sus-
pension. At 100 RPM, it is interesting to note how, due its shape,
the standard impeller creates two layers of rubber on top and 3. Calibration procedure
bottom. Thus, there is a clear evidence of phase separation in this
instance. On the contrary, the DHI creates a convective like flow The principle of operation of a rotational viscometer is to drive a
and it was visible how the inner thread raises up the rubber impeller, immersed in the test fluid. Torque is transmitted through
while the outer helps the particles to go downwards. As a result a calibrated spring. The viscous drag of the fluid against the impel-
of this, particles are suspended and move vertically, this permits a ler is measured by the spring deflection. Spring deflection is mea-
homogeneous distribution of RTR crumbs all over the blend even sured with a rotary transducer. Two Brookfield DV-II PRO Digital
after 20 min. Viscometers, a low torque (LV model) and high torque (HA model)
This preliminary study shows that rotational speed is an were used within this study. The two rotational viscometers differ
important factor in determining the efficacy of the impeller. Fur- mainly for the viscosity measurements range. The LV model is de-
thermore, the viscosity readings (not reported at this stage) are signed for low viscosity fluids (100% torque = 673.7 dyne cm),
shown to be stable despite the shape of the impeller and the while the HA model is more appropriate for medium–high viscous
heterogeneity of the sample. Thanks to these encouraging results, fluid (100% torque = 14,374 dyne cm) [29]. Torque measurement
the authors decided to proceed with the manufacture of a stain- accuracy specified by manufacturer is 1% of the full-scale range.
less steel DHI and its calibration to obtain reliable viscosity Two silicon standard viscosity Newtonian fluids were used for
measurements. calibration in this study. The two calibration fluids are indicated

Fig. 4. Preliminary study: begin.

274 D. Lo Presti et al. / Construction and Building Materials 67 (2014) 270–278

Fig. 5. Preliminary study: after 15 min (SC27), 20 min (DHI prototype).

Fig. 6. DHI manufacturing process: design, rapid prototyping through FDM and final tool produced with EDM.

from now on as fluid A and B, with viscosities at 25 °C of 99.6 cP In Eq. (1) SRC is the shear rate constant to be determined for
and 960 cP respectively. Viscosity measurements were carried each impeller geometry.
out on both the standards fluids by using a Thermosel Impeller The Brookfield viscometer automatically calculates the applied
SC-27 and the new dual helical impeller in order to perform the shear rate through Eq. (1). In particular an SRC value is associated
calibration procedure. Once the new impeller was calibrated, vis- with each impeller in order to calculate the shear rate, the shear
cosity measurements were carried out on 40/60 pen bitumen and stress and then the viscosity of the test fluids. If a non-standard
on a RTR-MB. impeller is used, a calibration procedure has to be performed to
determine the corresponding SRC value. The mathematical expres-
3.1. Theoretical considerations sions of the operating parameters found on various Brookfield
viscometers are stated in Eqs. (2)–(4):
Bitumens are found to be non-Newtonian with viscosity values
varying with the shear rate. This implies that the effective viscosity 2xR2s R2c
of the non-Newtonian fluid varies from point to point in the mixing
c_ ¼ ð2Þ
x2 ðR2c  R2s Þ
vessel. Then the knowledge of the shear rate distribution is central
to evaluate the viscosity of the fluid. But the complex flow field
created by the helical impeller in the mixing vessel is not known T
s¼ ð3Þ
a priori and does not allow to easily estimating the shear rate dis- 2pR2s L
tribution. This issue may be ameliorated by defining an average
shear rate value corresponding to an apparent viscosity value that T
can be determined as suggested by the Metzner and Otto method g¼ _ ð4Þ
c
[30]. Within this simplified approach the average shear rate c_ in
the measuring vessel is assumed to be proportional to the impeller
where w is the angular velocity of impeller (rad/s)[=(2p/60) N], N is
speed N and independent on the rheology of the fluid as shown in
the rotational speed (rpm), Rc is the radius of container (cm), Rs
Eq. (1).
is the radius of impeller (cm), x is the radius at which shear rate
is being calculated (cm), M is the torque input by instrument
c_ ¼ SRC  N ð1Þ (N cm), L is the effective length of impeller (cm).
 D. Lo Presti et al. / Construction and Building Materials 67 (2014) 270–278 275

The above mentioned equations apply to cylindrical geometries low shear mixer (§4.3). Fig. 9 shows the results of the viscosity mea-
only. In particular Eq. (2) is currently used in the calibration proce- surements at different rotational speeds by using both the SC-27
dure of non-standard impellers which conforms to cylinder or and the DHI impellers.
coaxial cylinder geometry. In this procedure the shear rate is first
calculated by means of Eq. (2) for a certain impeller speed and then 4.2. Viscosity measurements on recycled tyre rubber modified bitumen
the SRC is calculated by applying Eq. (1). However, the same proce-
dure cannot be applied for the dual helical impeller since it is not After the positive tests performed on the standard viscosity flu-
conformed to a cylindrical geometry. Therefore, an alternative pro- ids and on neat bitumen, the DHI has been used to measure the
cedure based on a robustness analysis to evaluate the appropriate apparent viscosity of a RTR-MB containing 15% of 30# RTR and pro-
SRC value for the new helical impeller, is proposed in the next duced in high shear. The tests have been performed in both LV and
section. HA models of rotational viscometers and compared with measure-
ments undertaken with the SC-27 impeller. According to the Stan-
3.2. Robustness analysis dard specification for Asphalt Rubber (ASTM D 6114-97), the
apparent viscosity measurement of the modified binder has to be
Viscosity measurements were carried out with both the stan- performed at 177.5 °C with a rotational speed of 12 RPM for LV
dard fluids by using the standard impeller SC-27 provided by the models and 20 RPM for the HA model. Measurements have pro-
Brookfield and the DHI. The tests were performed at a temperature duced similar results with both viscometers, so for the sake of sim-
of 25 °C while viscosity and torque values were measured with plicity Fig. 10 reports only the results obtained with LV viscometer.
varying rotational speeds. From Fig. 7, it can be observed that SC-27 impeller provides mea-
Measurements with the DHI were carried out with three differ- surements which pass through a wider transition period before
ent sets of measurements, each of them by setting a different SRC achieving a stable measurement, while DHI allows measurements
value. In particular the SRC value corresponding to the standard with a more stable trend. This could be explained by the capability
impeller SC-27, SC-28 and SC-29 have been chosen. The diameters of the DHI to create a convective flow within the sample which al-
of the three before mentioned impellers are respectively equal or lows reducing the initial effort needed to accelerate the bitumen–
smaller to the diameter of the external helix of the DHI. Figs. 6 rubber blend from a stationary position to a uniform shear speed.
and 8 show the measured viscosity values taken at different rota- It is well known that for non-homogenous fluids subjected to
tional speeds, respectively for fluid A and B. The average value and turbulent flow, the shear rate can affect viscosity measurements.
the mean square error (MSE) of the measured viscosity have been Furthermore, considering the eventual use of the DHI as impeller
calculated for each set of measurement and for each viscometer. to produce RTR-MB, by adapting the rotational viscometer as a
Results are detailed in Table 1. As previously discussed, the calibra- low shear mixer, also measurements at higher rotational speed
tion procedure has been performed on both LV and HA viscome- (50 and 100 RPM) have been performed.
ters. Results are shown to be comparable, therefore only those Due to the expected higher torque, only the HA model was used
related to the LV viscometer are here reported. in this phase. Fig. 11 shows that the transition period toward a sta-
Figs. 6 and 8 show also that the SRC value of 0.28 provides the ble measurement is similar for all the combination of speed and
best approximation to the true viscosity value for both the tested impellers. However, the initial effort needed to accelerate the bitu-
fluids. Furthermore, the corresponding average value of the mea- men–rubber blend is reduced when the DHI is used. Furthermore,
sured viscosity is close to the true one and the mean square error it has to be noticed that DHI shows almost uniform results also
is rather small as shown in Table 1. Therefore the SRC value of 0.28 changing shear speed, while SC-27 impeller shows higher suscep-
has been chosen as the shear rate constant of the DHI. tibility to the variation of the rotational speed. At last it has to be
highlighted, that at both high speeds DHI provides a lower appar-
4. Validation of results ent viscosity value which is 40% less of that measured by using the
standard SC-27 impeller.
4.1. Measurements on a 40/60 bitumen
4.3. Adapting the rotational viscometer as a low-shear mixer by using
Once the DHI was calibrated and the most reliable SRC had been the DHI
determined, viscosity measurements were carried out on a 40/60
pen bitumen at two test temperatures of 135 °C and 177.5 °C. The A previous study [25], has demonstrated the possibility of
first temperature is identified by the ASTM D4402 standard as the adapting a Brookfield rotational viscometer as a low shear mixer.
level at which characterising the viscosity of a bitumen at elevated This practical protocol allows constant monitoring of the viscosity
temperatures. The latter is the temperature suggested by the stan- of the binder, with accurate control of the temperature, and it
dard specification for Asphalt Rubber (ASTM D 6114-97), to assess offers the opportunity of understanding what is physically
the apparent viscosity of the binder, and it is also the temperature occurring during the process by monitoring the key parameter,
that has been used within this study to adapt the viscometer as a rotational viscosity. Furthermore, the protocol offers the chance

Fig. 7. Viscosity measurements by using LV viscometer on standard fluid 99.5.

276 D. Lo Presti et al. / Construction and Building Materials 67 (2014) 270–278

Fig. 8. Viscosity measurements by using LV on standard fluid 960.

Table 1
MSE and average value of the measured viscosity for fluid A and fluid B.

Fluid A SC-27 SRC = 0.34 DHI SRC = 0.34 DHI SRC = 0.28 DHI SRC = 0.25 Fluid B SC-27 SRC = 0.34 DHI SRC = 0.34 DHI SRC = 0.28 DHI SRC = 0.25
MSE 0.004 0.66 0.005 0.25 MSE 0.004 1.502 0.025 0.216
Average 93.7 54.42 98.93 200.86 Average 910.427 437.175 855.8129 1803.204

Fig. 9. Viscosity measurements by using LV on a 40/60 bitumen at T = 135 °C and 177.5 °C.

Fig. 10. Apparent viscosity of a TR-MB at 177.5 °C by using LV viscometer at 12 rpm.

Fig. 11. Apparent viscosity of a TR-MB at 177.5 °C by using HA viscometer at 50–100 rpm.
 D. Lo Presti et al. / Construction and Building Materials 67 (2014) 270–278 277

Fig. 12. Results of constant monitoring using the Brookfield viscometer as a low shear mixer at 177.5 °C.

to study the change in rheology of RTR-MBs blended with differ- viscometer as a low shear mixer and to guarantee more realistic
ent base binders, or different TR content, by drastically reducing viscosity measurements of samples which contains suspended par-
the material and time consumption. It is to be noticed that the ticles. The DHI geometry was designed to create a convective like
procedure allows producing a maximum of 15 g of modified bitu- flow within the sample which allows the uniform distribution of
men for further tests. This quantity is not enough to perform con- suspended solids within a low viscosity fluid. The results have
ventional tests like penetration, but it results to be sufficient in highlighted that:
order to perform Dynamic Mechanical Analyses (DMA) with a
DSR. However, the adaptation of a Brookfield viscometer with stan-  Layer based manufacturing techniques are shown to be a conve-
dard impellers is not trivial. In fact, as shown before in Fig. 5, the nient method to for rapid prototyping of complex geometries for
particular shape of the SC series impeller causes a phase separation surface–fluid interaction. This method also brings with it the
with some of the rubber particles settling down and most of them benefits of reduced cost of testing and accelerated lead times.
accumulating on the top of the sample. This phenomenon does not  The robustness analysis, conducted as calibration procedure for
allow having a homogenous distribution of rubber particles within low viscosity and high viscosity Brookfield viscometers, and the
the binder and so moving the impeller up and down during the validation of results showed that using the DHI with a shear
mixing, is necessary to help distribution of the rubber particles. rate constant of 0.28 (impeller 28), provides reliable viscosity
Fig. 12 shows the curve of the real-time apparent viscosity mea- measurements of homogenous fluids.
surements produced by mixing a 40/60 pen base bitumen with 15%  DHI provides similar results than the cylindrical standard
of 30# RTR crumbs (max diameter = 0.5 mm). The mixing process impeller (SC-27) only with the neat bitumen. In fact, by testing
has been performed at 177.5 °C, and 100 rpm for both SC-27 and the non-homogenous binder, RTR-MB, the DHI showed always
DHI impellers. A total time of 2 h and 30 min has been necessary lower values of apparent viscosity but with a more stable trend.
to obtain the peak viscosity with both impellers. Analysing the This could be explained by the capability of the DHI to create a
curve obtained by using the standard impeller, peaks are present convective like flow within the sample which allows reducing
at about 1000 and 2500 s. These are due to the manual lifting of the initial effort needed to accelerate the bitumen–rubber blend
the impeller to prevent the accumulation of rubber particles on from a stationary position to a uniform shear speed.
top of the sample. This is clear evidence of phase separation which  DHI is a feasible and improved solution for optimising the lab-
occurs when the impeller SC-27 is used to produce TR-MBs. It has oratory production of RTR-MB by adapting the rotational vis-
to be noticed that this manual moving of the impeller could lead to cometer as a low-shear mixer.
damage of the equipment.  Further studies are necessary to better understand the nature of
Mixing bitumen with RTR by using the DHI shows that the the convective like flow created by the DHI and to optimise its
helical impeller is a feasible solution for optimising the laboratory shape with regards to different viscosities range. However,
production of RTR-MB in low shear. In fact, there was no need of results obtained in this study show that an impeller with a dual
moving the impeller during the mixing because no accumulation helical shape could leads to more realistic viscosity measure-
of rubber particles on the top of the sample took place. However, ments of any fluids with suspended particles.
DHI was raised as well at 1000 s and 2500 s, but no evident
changes in viscosity have been noticed because the particles were
well distributed throughout the sample. Furthermore, Fig. 9 shows
that the viscosity value obtained with the DHI is always higher that References
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