Construction and Building Materials 36 (2012) 743–748

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Construction and Building Materials

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

A comparative study for improving the mechanical properties of cold

bituminous emulsion mixtures with cement and waste materials
Hassan Al Nageim a, Shakir Falih Al-Busaltan a,⇑, William Atherton a, George Sharples b
a
School of Built Environment, Liverpool John Moores University, Liverpool, UK
b
School of Pharmacy and Biomolecular Sciences, Liverpool John Moores University, Liverpool, UK

h i g h l i g h t s

" CBEMs are offering economic, environmental and safe application for pavements.
" FA has proved alternative to OPC in terms of mechanical and durability properties.
" New CBEMs’ mechanical and durability properties are comparative to traditional HMA.

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

Article history: This paper reports the experimental test results of a research project aimed at developing a new cold
Received 23 March 2012 bituminous emulsion mixtures (CBEM’s) containing fly ash from incinerated domestic and industrial
Received in revised form 23 May 2012 by-products compared with those results of traditional control cold containing OPC and hot mix asphalt.
Accepted 4 June 2012
The main objectives of the experiments were to investigate the improvement in mechanical properties
Available online 15 July 2012
of CBEM’s due to incorporating OPC, and detect the possibility of replacing the OPC with waste fly ash
materials. The mixtures mechanical properties investigated were; ITSM, creep stiffness. Durability in
Keywords:
term of water sensitivity was investigated too.
Cold bitumen emulsion mixtures
Fly ash
The results have shown comparative mechanical properties of CBEM’s to HMA. Furthermore, the new
Stiffness modulus CBEM’s with fly ash used as a replacement of filler achieved outstanding results compared with tradi-
Creep stiffness tional CBEM with and without addition of OPC. Therefore, this paper introduces a new CBEM’s having
outstanding mechanical characteristics, cost effective, and environmental friendly.
Ó 2012 Elsevier Ltd. All rights reserved.

1. Introduction materials to reach their full strength after paving, especially in

Cold mix asphalt is a bituminous material produces at ambient
temperatures. Several environmental and cost effective character-
istics can be obtained when cold mixes are underutilised rather
than traditionally hot mixes. But, these mixes have shown inferior
characteristics such as weak earlier-life mechanical properties and
high porosity compared with hot mix asphalt (HMA) [1,2].
Cold bitumen emulsion mixture (CBEM) is the most famous
type of cold mix asphalt. In UK and worldwide, the use of CBEM
is largely restricted to surface treatment such as surface dressing
slurry surfacing, and reinstatement work on low trafficked and
walkways [3–5]. Thus, uses of cold emulsified asphalt for structural
layers are very limited, due to the long time required for such
⇑ Corresponding author. Tel.: +44 7780145991.
E-mail addresses: h.k.alnageim@ljmu.ac.uk (H. Al Nageim), s.f.al-busal-
tan@2010.ljmu.ac.uk, shakerfa2003@yahoo.com (S.F. Al-Busaltan), w.atherton@lj-
mu.ac.uk (W. Atherton), G.P.sharples@ljmu.ac.uk (G. Sharples).
the UK climate. In addition, such mixes are highly sensitive to rain-
fall at early life [6,7].
Mechanical properties of bituminous pavement including; stiff-
ness modulus, permanent deformation and fatigue resistance are
affected by many factors such as; based binder grade and charac-
teristics, mixture void content, curing time, aggregate characteris-
tics, and additives [1,8]. Attempts to improve cold mixes
mechanical properties have been investigated by several research-
ers such as Head who had indicated that Marshall Stability of mod-
ified cold asphalt mix increased by 250–300% with the addition of
1% ordinary Portland cement (OPC) compared with un-treated mix
[9]. Oruc et al. conducted experiments to evaluate the mechanical
properties of emulsified asphalt mixtures having 0–6% Portland ce-
ment [2]. Their test results showed significant improvement with
high Portland cement addition percentage; moreover they sug-
gested based on the study test results, that the cement modified
asphalt emulsion mixes might be used as structural pavement
layer. Thanaya et al. reported the test results of research on cold

0950-0618/$ - see front matter Ó 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.conbuildmat.2012.06.032
744 H. Al Nageim et al. / Construction and Building Materials 36 (2012) 743–748

Table 1 are mostly industrial by-products. Thirdly, trapped water could

Aggregate grading for 0/10 mm size close graded surface course BS EN 4987-1. be reacted with these materials to complete the hydration process
Test sieve aperture size Mass passing specification Mass passing mid and the result is getting rid of this water which is the main reason
(mm) range (%) (%) of increasing the curing period in cold mix asphalt, and lastly, the
14 100 100 ecological benefit factor.
10 95–100 97.5 A research works implemented by Thanaya et al. indicated that
6.3 55–75 65 the pulverised fly ash (PFA) can be used as suitable filler in cold
2 19–37 28
1 10–30 20
mixes at full curing conditions [13]. Also they found that the fully
0.063 3–8 5.5 cured stiffness of cold mix achieved is very comparable to hot
mixtures.
The central theme of the work reported here concerns the use of
upgraded fly ash (FA) generated from domestic and industrial by-
Table 2
product as filler in cold bitumen emulsion mixtures to overcome
Physical properties of aggregates. the problem of inferiority of cold mix, namely low tensile stiffness
and creep stiffness. Previous studies mentioned above prove that
Properties Value
ordinary Portland cement, rapid setting cement and other addi-
Coarse aggregate tives improved the mechanical properties of CBEM’s, but they have
Bulk specific gravity (g/cm3) 2.79
the disadvantage of high cost and other related environmental
Apparent specific gravity (g/cm3) 2.82
Water absorption (%) 0.4 impacts.
The upgraded FA which is used in this research is boiler ash res-
Fine aggregate
Bulk specific gravity (g/cm3) 2.74 idue resulting from incineration of waste sludge in energy produc-
Apparent specific gravity (g/cm3) 2.77 tion. Annually, millions of tonnes of FA are generating in UK and
Water absorption (%) 0.4 world wide. FA main ingredients are CaO, SiO2 and Al2O3. There-
fore, pozzolanic reaction must be generated when mixed with cold
mixture components. On the other hand, FA has other advantage as
it has high water absorptive, and therefore this filler named as in
emulsion mixtures [10]. They showed that the addition of 1–2% ra- the following section of research FA is useful for absorbing trapped
pid-setting cement accelerate the earlier strength as well as im- water in CBEM’s.
prove the mechanical performance of the modified cold mixes. The developed CBEM’s in this study incorporate percentage FA
Pouliot et al. conducted a study with the aim of understanding as a filler replacement in the mix with varying from 0% to 5.5% of
the hydration process, the microstructure, and the mechanical the aggregate weight. The improvement in mechanical properties
properties of mortars prepared with a new mixed binder made of determined using the indirect tensile stiffness modulus and uniax-
a cement slurry and a small quantity of asphalt emulsion (SS-1 ial compressive cyclic test, as a respected indicators of the mechan-
and CSS-1) (i.e. anionic and cationic emulsion) [11]. They proved ical properties. At the same time, water sensitivity test was used to
that the presence of a small quantity of emulsion had an effect investigate the durability of the new mixes.
on the cement hydration. Their test results also indicated that
the launch of asphalt droplets inside a cement mortar matrix leads
to a considerable reduction in compressive strength and elastic 2. Materials and methods
modulus in addition to a slight decrease in flexural strength. Also,
2.1. Materials
they found that the cationic emulsion (CSS-1) in contrast with an-
ionic emulsion (SS-1) shows higher mortars strengths and elastic The aggregate used in this study is crushed green granite from Cliffe Hill quarry
modulus. Other study by Wang and Sha indicated that the increase and the aggregate gradation is given in Table 1. Physical properties of the aggre-
of cement and mineral filler fineness has a positive impact on mi- gates are given in Table 2. The aggregate were dried, riffled and bagged with sieve
analysis achieved in according with BS EN 933-1 [14] and BS EN 12697-28 [15]. In
cro hardness of the interface of aggregate and cement emulsion order to ensure appropriate interlocking of the close graded surface course, mix gra-
mortar [12]. However, the use of very fine mineral filler is disad- dation was selected according to BS EN 4987-1 [16], 0/10 mm close graded surface
vantageous. Furthermore, they showed that the limestone and course gradation have been used in this research work.
limestone filler impact hardness values high when compared with The selection of this gradation is due to the fact that this gradation has been
used successfully in the heavy traffic surface coarse hot coated macadam [16]. Also,
granite and granite filler’s.
The dense gradation has much coarse aggregates portion compared with close gra-
Other attempts tried the use of waste and by-products materi- dation, and according to Doyle et al., the more the coarse aggregate grading in the
als to improve cold mixes, where four main benefits can be mix the less compactability and specimens disintegrated upon extrusion [17].
achieved when utilising the by-product materials on CBEM’s. Cationic slow setting bitumen emulsion (K3) was selected for cold mixes to en-
Firstly, improving mechanical properties, in general there will be sure high adhesion between aggregates particles. While, 143 and 53 pen grades
bituminous binder were selected for soft and hard hot mix asphalt. Table 3 shows
an enhancement of ultimate strength due to the cementitious the properties of the selected emulsion. Three types filler were used traditional
properties of the added waste materials. Secondly, gaining eco- mineral filler, OPC and FA. Table 4 shows the chemical composition of the fillers
nomic benefit as the pozzolanic and cementitious materials used used in this research work.

Table 3
Bituminous binder and bituminous emulsion properties.

Bitumen emulsion Bituminous binder 100–150 Bituminous binder 40–60

Properties Value Properties Value Properties Value
Appearance Black to dark brown liquid Appearance Black Appearance Black
Boiling Point (°C) 100 Penetration 25 °C 143 Penetration 25 °C 43
pH 5 Softening point (°C) 43.6 Softening point (°C) 52.4
Relative density at 15 °C g/ml 1.05 Kinematic viscosity at 135 °C 175 Kinematic viscosity at 135 °C 325
Residue by distillation (%) 56 Density at 25 °C 1.00 Density at 25 °C 1.01
 H. Al Nageim et al. / Construction and Building Materials 36 (2012) 743–748 745

Table 4 with 50 blows to each face of the specimens. Moreover, conventional hot mixture
Chemical composition of fillers. samples were prepared with the same aggregate type and gradation, 5.3% binder
content was used to match the requirements of BS EN 4987 2005 for 0/10 mm size
Element Concentration close graded surface course-preferred mixtures. Both cold and hot mixes were pre-
Mineral filler OPC FA pared in quantity to produce three 1100 gm specimens for each specific mix. Mix
type and the percentages of the filler used are shown in Table 5. The cold mix spec-
CaO 5.58 63.25 60.93 imens were mixed and compacted at lab temperature (20–25 °C), while hot mix
SiO2 53.597 25.61 28.178 specimens were compacted at (135–140 °C).
Al2O3 9.221 2.15 3.471
MgO 4.984 1.52 3.554
Fe2O3 7.368 1.08 0.202 2.3. Samples conditioning
K2O 3.123 0.77 0.354
TiO2 0.831 0.34 0.556 Cold mixtures strength characteristics are very sensitive to curing time and
temperature. Therefore and as can be seen in Table 6, samples curing conditioning
for the different tests were achieved at two stages. First stage where the sample
needs to be left in mould before extruded is to prevent specimen disintegration.
Second stage is to identify Mixture properties to specific age. The selections of sec-
ond stage criteria based on the past curing criteria adopted by various researchers;
Table 5
Jerkins provided a comprehensive overview of these curing criteria for foamed bitu-
Mixtures matrix.
men asphalt [20]. He reported that 24 h @ 20 °C plus 24 h @ 40 °C represent 7–
Mix type Filler 14 day. Generally for ITSM, five specimens were prepared and tested to represent
each single test result with a standard deviation not more than 108 MPa.
CBEM-1 5.5% conventional mineral filler For uniaxial compressive cyclic test, the curing conditioning was selected
CBEM-1O 1.375% OPC according to Thanaya recommendations [8], whereas the specimens placed in an
CBEM-2O 2.75% OPC oven for 14 days at 40 °C to make sure it reached its full curing condition. Generally
CBEM-3O 4.125% OPC for UCCT, five specimens were prepared and tested to represent each single test re-
CBEM-4O 5.5% OPC sult with a standard deviation for the strain at the end of the test not more than 759
CBEM-1F 1.375% FA microstrain. On the other hand, curing of durability test samples have been
CBEM-2F 2.75% FA achieved according to BS EN 12697-12 [21]. While five specimens were prepared
CBEM-3F 4.125% FA and tested to represent each single test result for durability test, with a standard
CBEM-4F 5.5% FA deviation not more than 110 MPa.
HMA-1 Traditional hot mix asphalt 143 penetration asphalt binder
HMA-2 Traditional hot mix asphalt 53 penetration asphalt binder
3. Testing and results

2.2. Mix design and sample preparations 3.1. Experimental tests

At the moment, there is no UK, or universally accepted design mixture for the
CBEM’s. So all samples produced for this study was prepared according the method
adopted by the Asphalt Institute (Marshall Method for Emulsified Asphalt Aggre-
gate Cold Mixture Design (MS-14)) [18]. Only one change has been done to the said
method by replacing the Marshall test with the indirect tensile strength. The design
method and sample preparations achieved through the following steps:
 Determine the aggregate gradation: the selection of the aggregate gradation
have been done as mentioned in Section 2.1
 Determine the initial emulsion content: an empirical equation which depends
on the aggregate gradation was used as recommended by Asphalt institute
manual MS-14
 Determine pre-wetting water content: coating ability of the bitumen emulsion
to the aggregates is highly sensitive to the pre-wetting water content, especially
when the aggregate gradation containing a high percentage of materials passing
a 63 lm sieve. Thanaya was reported that inadequate pre-wetting water con-
tent results in balling of the binder with fines portion of the aggregate and thus
unsatisfactory coating [8]. Different pre-wetting water contents investigated to
find the lowest percentage to ensure adequate coating.
 Optimum emulsion content: indirect tensile strength test is used to determine
the optimum emulsion content according to BS EN 12697-23 [19].
 Determine the optimum total liquid content: the mix density test was used to
determine the optimum total liquid content at compaction (i.e. emulsion plus
pre-wetting water contents which give highest mix indirect tensile strength
and density).
Three fundamental tests were used to identify the mechanical
properties of CBEM’s and HMA. These tests are as follows:
 Indirect tensile stiffness modulus (ITSM): The test was con-
ducted in accordance with BS EN 12697-26 [22], using Cooper
Research Technology HYD 25 testing apparatus. The test condi-
tions as in Table 7.
 The uniaxial compressive cyclic test (UCCT): The test was con-
ducted in accordance with BS EN 12697-25 [23], using Cooper
Research Technology HYD 25 testing apparatus. The test condi-
tions as in Table 8.
 Durability (water sensitivity) test: The test was conducted in
accordance with BS EN 12697-12 [21]. Modification has been
made by determine stiffness modulus ratio (SMR) instead of
Indirect Tensile Strength Ration (ITSR). The Cooper Research
Technology HYD 25 testing apparatus was used. The test condi-
tions for this test are similar to indirect tensile stiffness modu-
lus test.
3.2. Results and discussion

Therefore, according to the selected materials characteristics, pre-wetting water
content was observed to be 4%, the optimum bitumen emulsion was 11.5% and opti-
mum total liquid content at compaction was 14.5% of aggregate weight.
Specimens of cold bitumen emulsion mixtures were prepared using different
amounts of OPC and FA as a replacement of mineral filler ranging from 0% to
5.5% of total aggregate weight. Impact compacting (Marshall Hammer) was applied
3.2.1. Indirect tensile stiffness modulus
The results of the indirect tensile stiffness modulus tests are
shown in Figs. 1–4 for CBEM’s specimens with HMA results for
compression. Specimens were tested at age of 2,7,14, 28, 90, 180
and 360 days.

Table 6
CBEM’s curing protocol.

Test First stage curing Second stage curing Time testing (days) Recommended by
Indirect tensile stiffness modulus 20 °C for 1 day 40 °C for 1 day 2,7,14,28,90, 180 and 360 days [20]
Uniaxial compression cyclic 20 °C for 1 day 40 °C for 14 days 15 [8]
Stiffness 20 °C for 1 day 20 °C for 9 days 10 BS EN 12697-12 [21]
Modulus ratio (durability test) 20 °C for 1 day 20 °C for 6 days, then socked 3 days at 30 °C
746 H. Al Nageim et al. / Construction and Building Materials 36 (2012) 743–748

Table 7 360 days the rate of increase in ITSM values is relatively small
ITSM test conditions. compared with its values at early stage. In contrast the HMA
Item Range showed no significant change with time. Additionally, the rate of
Specimen diameter (mm) 100 ± 3
Rise time 124 ± 4 ms
Transient peak horizontal deformation 5 lm
Loading time 3–300 s
Poisson’s ratio 0.35
No. of conditioning plus 10
No. of test plus 5
Test temperature (°C) 20 ± 0.5
Specimen thickness (mm) 63 ± 3
Compaction Marshall 50  2
Specimen temp. conditioning 4 h before testing

Table 8
UCCT conditions.

Item Range
Frequency 0.5 Hz
Loads 100 ± 2 kPa
Loading pulse 1 ± 0.05 s Fig. 3. ITSM of CBEM’s for OPC and FA at 2 days.
Rest period 1 ± 0.05 s
Preloading 10 kPa for 10 min
Poisson’s ratio 0.35 for 20 °C test temp.
No. of test plus 3600
Test temperature (°C) 40 ± 0.5
Specimen diameter 148 ± 5
Specimen thickness 60 ± 2 mm

Fig. 4. ITSM of CBEM’s for OPC and FA at 7 days.

Fig. 1. Effect of % OPC on ITSM.

Fig. 5. Accumulative creep strain versus pulse count of specimens with different %
of filler.

Fig. 2. Effect of % FA on ITSM.

The results of ITSM of CBEM’s comprised OPC are shown in

Fig. 1. The results indicate that the stiffness modulus increased sig-
nificantly at early stage, namely from 2 to 28 days. At age of 28– Fig. 6. Effect of % of filler on creep stiffness.
 H. Al Nageim et al. / Construction and Building Materials 36 (2012) 743–748
Creep Rate (microstrain/loading
pulse)
Fig. 7. Effect of % filler on creep rate.
increase in the CBEM’s stiffness modulus increases as the OPC per-
centage increases. However, CBEM’s stiffness modulus reached the
soft HMA’s (143 pen) stiffness levels with high OPC content of
more than 4.125% and after few days, whereas these CBEM’s Mix-
tures stiffness need few months to reach hard HMA’s (53 pen)
stiffness.
On the other side, the results of ITSM of CBEM’s comprised FA
showed also a significant increment in ITSM with time (Fig. 2) with
similar behaviour to that of mixtures comprised OPC (Fig. 1) with
relatively highest values. The results reveal an outstanding stiff-
ness modulus values in contrast with CBEM’s comprised OPC and
HMA.
For continuing comparison purposes, Figs. 3 and 4 illustrate the
ITSM results for specimens for 2 and 7 days respectively. The selec-
tion of these times to prove the ability of such mixtures to with-
standing traffic loads within acceptable times. Firstly, the result
shows that CBEM’s comprised FA gives highest ITSM that CBEM’s
with OPC, where the increment rate is ranged between 2% and
60%. Secondly and for the first time, CBEM’s contained FA can be
Fig. 8. Effect of OPC % on stiffness modulus ratio.
Fig. 9. Effect of FA % on stiffness modulus ratio.
747
an alternative for HMA as stiffness modulus reach a comparison
value within 2–7 days which is in fact represent 7–14 days in rel-
evant weather [20].
The replacement of the conventional mineral filler in CBEM’s
with a filler which has cementitious properties such as OPC or FA
developed an outstanding improvement in CBEM’s mechanical
properties and reduces the curing time to reach the material ulti-
mate strength. These improvements are due to the fact that the
majority of the trapped water between aggregate and residue bin-
der was absorbed by the replacement filler. The increase in ITSM is
highly depends on both the water absorbability of filler materials
and its reactivity with water and resulting in a secondary binder
formed as a results of the hydration process of cementitious filler
in the present of water beside the residual asphalt binder. Both
binders form a strong bitumen–cement paste binding the CBEM’s
internal texture.
3.2.2. Uniaxial compressive cyclic test
The results of the uniaxial compressive cyclic tests are given in
Figs. 5–7 which confirm the following: (i) controlled CBEM with
conventional mineral filler failed after 1000 pulses which demon-
strates that the CBEM without cementitious filler has the smallest
resistance to permanent deformation compared to other mixtures,
(ii) the full cured CBEM’s specimens containing 2.75–5.5% cemen-
titious filler offered significantly high resistance to permanent
deformation and better than the soft and hard HMA, (iii) the resis-
tance to permanent deformation is increased by increasing the
cementitious fillers, (iv) the CBEM’s comprised FA offered better
permanent resistance than CBEM’s containing OPC. The said
improvement in ITSM results due to the addition of cementitious
filler has resulted in an improved resistance of the CBEM’s to per-
manent deformation.
748 H. Al Nageim et al. / Construction and Building Materials 36 (2012) 743–748
3.2.3. Durability – water sensitivity
The Durability of CBEM’s in terms of water sensitivity can be
achieved using either the indirect tensile strength ratio (ITSR) or
indirect tensile stiffness modulus ratio (SMR). As the load condi-
tions in the former test is more fundamental, the SRM was adapted
in this research study. The specimens were divided into two sets,
the first set of specimens (unconditioned) was cured at 20 °C for
10 days and the ITSM achieved. The second set of specimens, (con-
ditioned) was cured at 20 °C for 7 day and then the specimens sub-
jected to vacuum for 1 h before immersed in water path for 3 days
under 30 °C. Finally the ITSM for the second set was achieved and
the ratio of the conditioned ITSM to unconditioned is determined.
Results of the water sensitivity tests are shown in Figs. 8 and 9.
From these results the following can be stated: (i) CBEM’s com-
prised non or low cementitious filler (64.124%) showed high water
sensitivity; (ii) CBEM’s with more than 2.75% cementitious filler
showed positive effect, i.e. the SRM was more than 100%; (iii)
CBEM’s comprised FA offered better positive effect under water
sensitivity tests than the CBEM’s comprised OPC.
The hydration process and the development of the secondary
cementitious binder mentioned before are the main reasons for
the increase in ITSM of the conditioned specimens.
4. Conclusion
Based on the experimental results of this study, the following
can be concluded:
1. The low early stiffness modulus, creep modulus of conventional
CBEM’s together with its unacceptable water sensitivity can be
improved by using cementitious filler as a replacement of con-
ventional mineral filler.
2. The CBEM’s containing OPC cementitious filler offered stiffness
properties higher than the soft and hard traditional HMA at cur-
ing time of 14 and 125 days respectively.
3. The FA filler which is a waste material prove its significant
enhancing stiffness properties to CBEM’s compared with OPC,
plus the other characteristic such as cost and environment
impacts. CBEM’s containing FA offered stiffness properties
higher than soft and hard traditional HMA at curing time of 3
and 14 days respectively.
4. The superiority of the FA filler to OPC in enhancing the mechan-
ical properties of CBEM’s is due to its high water absorbability.
This subject is under investigation by the authors and will be
the subject for another paper to be published.
Acknowledgements
The authors wish to thank Dr. Linda Seton and Mrs. Nicola
Dempster from the School of Pharmacy and Biomolecular Sciences,
Liverpool John Moores University for their help and supports in
this research project.
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