Construction and Building Materials 128 (2016) 287–297

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Construction and Building Materials

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Sugar cane bagasse ash from a high efficiency co-generation boiler:

Applications in cement and mortar production
Elisabeth Arif a, Malcolm W. Clark a,b,⇑, Neal Lake a
a
School of Environment, Science and Engineering, Southern Cross University, PO Box 157, Lismore, NSW 2480, Australia
b
Marine Ecology Research Centre, Southern Cross University, PO Box 157, Lismore, NSW 2480, Australia

h i g h l i g h t s

Pozzolanic activity of these bagasse ashes is low and most beneficial as filler-materials.

Activity reduces from polymorph phase changes to a-quartz at high burn temperatures.

Increases in sulphuric acid resistance are displayed in compressive strength retention.

Acid resistance is reflected in significantly reduced mass loss from expansion, and spalling.

Acid resistance occurs from pore-filling and/or cement chemistry shifts from C3A, to C2S.

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

Article history: Sugarcane bagasse ash (SCBA) has been reported to be beneficial as cement replacement due to the poz-
Received 31 December 2015 zolanic and the filler effect. The SCBA from a high-efficiency (high temperature) co-generation boiler does
Received in revised form 28 September not contain significant amorphous silica rather it contains a-quartz generated by phase transitions during
2016
combustion. The high combustion temperatures appear to deactivate the silica, and lime-SCBA pastes
Accepted 19 October 2016
show little or no pozzolanic activity present, except at a 5% replacement. Compressive strength testing
of the cement pastes also suggests that at 5% cement replacement level, the SCBA is potentially poz-
zolanic. However, up to 15% SCBA cement replacements achieve a pozzolanic index above 75%, which
Keywords:
Sugar cane bagasse ash
suggests increases in pozzolanic activity by the relative strength tests are more likely from a filler effect
Pozzalanic reaction than true pozzolanic activity. Despite an apparent lack of pozzolanic activity all SCBA’s additions
Filler improved sulphuric acid resistance measured both through compressive strength testing and mass loss
Sulphate resistant measurements.
Co-generation boilers Ó 2016 Elsevier Ltd. All rights reserved.

1. Introduction and durability depending on the pozzolanic activity of the SCM

In concrete the binder is typically ordinary Portland cement
(OPC), which provides essential strength and durability. However,
cement production significantly contributes to global greenhouse
gas emissions through large volumes of carbon dioxide (CO2); 1
tonne of OPC releases 1 tonne of CO2 [1,2]. Consequently, one suc-
cessful method of reducing the environmental impact of concrete
has been partial replacement of OPC with supplementary cementi-
tious materials (SCMs) often sourced from industrial or agricultural
wastes [1,3]. SCMs not only improve the environmental credibility
of the concrete industry, but may also improve concrete strength
⇑ Corresponding author at: School of Environment, Science and Engineering,
Southern Cross University, PO Box 157, Lismore, NSW 2480, Australia.
E-mail address: malcolm.clark@scu.edu.au (M.W. Clark).
and the concrete [3].
An SCM must be pozzolanic in nature, defined as being silic-
eous, or siliceous and aluminous materials, which may not be nat-
urally cementitious, but react with calcium hydroxide (Ca(OH)2)
and water to form cementitious compounds [8]. A material may
be classed as a pozzolan if its strength activity index (SAI) is at least
75% [9], which is determined by comparing the compressive
strength developments between a mortar containing the potential
pozzolanic material and a control mortar [10]. A further chemical
requirement is that the mass percent of silica + alumina + iron
oxide (SiO2 + Al2O3 + Fe2O3) is above 50% for class C pozzolans
and above 70% for class F pozzolans [11]. Concrete durability in
acidic and other aggressive environments (e.g., sewage systems,
acid sulphate soils) can be prone to sulphuric acid attack, resulting
in rapid deterioration [4]. Hence, some SCMs have been shown to
improve the durability in these harsh environments [5–7], because

http://dx.doi.org/10.1016/j.conbuildmat.2016.10.091
0950-0618/Ó 2016 Elsevier Ltd. All rights reserved.
288 E. Arif et al. / Construction and Building Materials 128 (2016) 287–297
of the SCM pozzolanic consumption of Ca(OH)2 and aluminates.
Excess Ca(OH)2 and aluminate react with H2SO4 producing the
low density and expansive gypsum and ettringite, which leads to
cracking and spalling. Thus, incorporating SCMs in concrete
exposed to these aggressive environments not only reduces the
demand on cement production, but also reduces economic losses
due to repairs, maintenance and reduced service life [5]. Industrial
waste materials are often used as pozzolans including coal fly ash
(CFA) [12,13], granulated blast furnace slag (GBFS) [14], and the
agricultural wastes such as rice husk ash (RHA) [15,16] and sugar-
cane bagasse ash (SCBA) [17–29].
SCBA results from the burning of the cane bagasse (the organic
pulp after juice extraction) for the co-generated heat and energy at
a sugar mill. The heat and energy is used in the processing of the
sugarcane juice into raw sugar. Brazil, the world’s largest sugar-
cane cultivators, generate over 2.5 million tonnes of SCBA per
annum [30], whilst Australia generates some 230 thousand tonnes
[31]. The principle disposal methods for SCBA are dumping to land-
fill, or mixing with mill mud (dirt and solids washed from the cane,
and clarified from the cane juice) and returning to the cane field as
a low-level fertilizer. However, his latter practice is diminishing
because of environmental and health concerns [32] and the possi-
bility of alternative value added solutions. SCBA utilizations previ-
ously investigated include the use of it as an adsorbent [33,34],
glass-ceramic material production [35], geopolymers [36], and
zeolite production [37]. Furthermore, considerable research has
been conducted on SCBA waste utilization in the concrete industry,
where most of the work has focused on SCBA as either a cementi-
tious replacement [17,18,20–23,25,38,39], or as a filler [29,40].
SCBA differs slightly in chemical composition (Table 1) to the
common pozzolan CFA, but is also a fine particulate aluminosili-
cate ash. SCBA compositional variations do occur depending on
the plant growth conditions, bagasse combustion environment,
purity of the bagasse feed-stock, and also on the bagasse ash col-
lection point, for example ash collected from the bottom of the boi-
ler may contain greater amounts of coarse irregular particles and a
lower char content compared to ash collected from the boiler fil-
tration systems [23]. However, the predominance of silica is typical
(Table 1) with SCBA consistently containing some alumina and
minor quantities of additional metal oxides; SCBA is by definition
an aluminosilicate. Similarly, there are also varying amounts of
carbon contents (carbonates and un-burnt organic carbon) and
water, expressed as LOI.
Previous studies show that OPC replacement by SCBA at 20% by
weight of OPC increases the compressive strengths of concrete
[38,42], or at least obtain equivalent strength [24]. Similarly, mor-
tars with a 10% replacement level showed SAIs above the required
75% [25] and has also been shown to improve the sulphate resis-
tance [39] and sulphuric acid resistance [43]. Furthermore,
replacement in mortars up to 30% has been reported to develop
greater compressive strengths [39]. However others report that
Table 1
Chemical composition and LOI of sugarcane bagasse ash from varied sources compared to typical CFA composition.
Chemical compound (%wt) CFA SCBA
[41] [38]
SiO2 20–40 62
Al2O3 5–35 6.7
Fe2O3 10–40 5.8
CaO 1–12 6.2
MgO 0–5 3.0
SO3 0–4 0.72
Na2O 0–4 3.2
K2O 0–3 6.9
LOI 0–15 2.6
20% SCBA reduced 28 day compressive strength and that a 5%
replacement level was optimal [44]. Where SCBA as-received
showed poor strength development in concretes and mortars, that
various pre-treatments to the SCBA such as grinding improved the
pozzolanic activity [17–20], which suggest that ash reactivity is
variable, and individual to the boiler/furnace system. However,
studies that show a limited pozzolanic activity report the material
may still benefit concrete through filler effects by replacing sand
instead of binder [29].
Previous SCBA incorporation studies highlight the potential as a
beneficial replacement material in concrete, but that variations in
material lead to variations in the suitability of SCBA as an SCM
[23]. It is therefore vital that individual sources of SCBA be evalu-
ated in terms of chemical and physical characteristics to determine
the most effective utilization of this waste source. This paper
investigates the chemical and physical effects that local co-
generation plant SCBA has on lime-pozzolan binders, cement
pastes and mortars. Results from this study provide important
insights into the pozzolanic potential and acid resistance of SCBA
in concrete, and inform whether pre-treatment of the SCBA or
alternative utilizations are necessary.
2. Experimental program
2.1. Materials characterization
The cement used for all work was a general purpose (GP) ordi-
nary Portland cement manufactured by ‘Sunstate Cement’ and
complying with AS 3972 [45]. The SCBA used was obtained from
the Broadwater Sugar Mill Co-Generation Plant, NSW, was black
in color and used as received, except for oven drying at 105 °C to
remove free water. The chemical compositions of the cement and
the SCBA were determined using a PANalytical Epsilon 3 X-ray Flu-
orescence (XRF). Concentrations were calculated against Omnian
standards in Panalytical Epsilon3 Software; no matrix corrections
were applied, and data should be considered semi-quantitative.
Carbon and nitrogen concentrations were measured on a LECO
2000 Analyzer. The sample was bound with wax (9:1) and pressed
as a pellet for 30 s at 20 tonnes pressure. Reagent grade Ca(OH)2
was used in lime-pozzolan binder paste tests and distilled de-
ionized water was used in all tests. Mortar used a European Com-
mittee for Standardization (CEN) standard sand conforming to BS
EN 196-1 [46] and was supplied by Normensand and the specific
gravities of the cement and SCBA were determined using Le Chat-
lier flask in accordance with AS 3583.5 [47].
The particle size distributions of both the cement and the SCBA
were determined using a Malvern Mastersizer 2000 using ethyl
alcohol as a dispersant with 20 min of ultrasonic agitation. Particle
morphology was qualitatively determined using scanning electron
microscopy (SEM) on a Phenom XL DesktopTM SEM with integrated
energy dispersive spectroscopy (EDS) detector which was used for
[42] [17] [23]
54 78 67
5.7 8.6 9.5
3.5 3.6 10
15 2.2 1.4
1.4 1.7 0.92
0.03 ... 0.10
... 0.12 0.22
... 3.5 3.2
19 0.42 4.3
 E. Arif et al. / Construction and Building Materials 128 (2016) 287–297
elemental analysis of selected particles (Fig. 2). The SEM was per-
formed at an acceleration voltage of 10 kV using uncoated samples.
The mineralogical properties of the SCBA were determined using
X-ray diffraction (XRD). Samples were milled to a powder
(<10 lm) prior to scanning by a Bruker D4 Endeavor XRD with a
Lynxeye position sensitive detector. Cobalt Ka1 radiation was used
at 40 kV and 40 mA over a range of 5° and 80° 2h, with a step size of
0.03572° 2h and 1.65 s/step.
2.2. Mix proportions
Lime-SCBA pastes were made with 50% lime and 50% SCBA (by
weight) with a water to solid ratio (by weight) of 0.6. The lime con-
tent of the resultant paste was then measured using XRD analysis
to determine the pozzolanic properties of the SCBA at 1, 7 and
28 days. Compressive strength testing of 50 mm lime-SCBA paste
cubes were determined at 1, 7 and 28 days.
Five cement paste mixes were made by replacing increasing
weights of cement with SCBA including a control (0%), 5%, 10%,
15% and 20%. For each paste, water was added to maintain a ‘‘nor-
mal consistency” (Table 2), as determined in accordance with
AS2350.3 [48]. Testing included the initial and final setting time
[49], the pozzolanic activity index by comparison of the compres-
sive strengths of 50 mm cubes at 1, 7, and 28 days and examination
of the pozzolanic activity using XRD analysis of the 1, 7, and 28 day
hardened cubes [50].
Mortars, to investigate the pozzolanic index and relative water
requirements with increasing SCBA content, were based on the
standard mortar mix [10] where 450 ± 2 g cement and 1350 ± 5 g
of CEN standard sand was used adding the weight of water neces-
sary to achieve a 110% flow on the flow table [51] (Table 3). SCBA
was used to replace the cement at 0, 5, 10, 15, & 20% by mass.
2.3. Manufacturing and curing of specimens
An automatic bench mounted mixer ‘Auto-Mortar MixerTM’ was
used in the preparation of all samples. For lime and cement pastes
the dry ingredients were first added to the stainless steel mixer
bowl and combined until homogenized. Water was then added,
followed immediately by mixing for 75 s on low speed (140 r/
min), resting for 15 s and a further final mixing on low for 60 s
[49]. Mortar mixes had the cement and SCBA first added to the
bowl and homogenized, followed by water addition and mixing
on low for 30 s. The CEN standard sand was then added over the
next 30 s followed by 30 s mixing on high speed (285 r/min). The
mortar mix was then allowed to rest for 90 s followed by a further
60 s of high speed mixing [52]. Both Lime-SCBA pastes and
cement-SCBA pastes were cast into 50 mm cubes. A total of 9
lime-SCBA cubes and 45 cement-SCBA pastes cubes were pro-
duced. A total of 15 mortar specimens for the pozzolanic index
study were cast into 40 mm  40 mm  160 mm prisms for
28 day compressive strength tests [10]. The determination of acid
resistance was conducted for the mortar using 90 specimens cast
into 50 mm cubes, with half the specimens exposed to acid and
the remainder used as the control.
Table 2
Mix proportions of cement-SCBA pastes.
Mix Designation GP Cement (g) SCBA (g) Water (g)
CP0A 600 0 177.0
CP5A 570 30 200.0
CP10A 540 60 222.5
CP15A 510 90 237.5
CP20A 480 120 255.0
289
All specimens were maintained in moulds in a controlled envi-
ronment room at 23 °C, with a relative humidity of 90% for 24 h.
Mortars and cement-SCBA pastes were then demoulded and placed
in a lime saturated curing tank maintained at 23 ± 2 °C until the
time of testing. After demolding the lime-SCBA pastes remained
in the environment room wrapped in plastic until testing. All spec-
imens tested at 1 day were tested immediately after removal from
the mould. Mortars that were placed in acid solution were first
cured in the lime saturated curing tank until they reached 7 day
age.
2.4. Test methods
2.4.1. Lime and cement pastes
Lime-SCBA paste specimens were first tested for compressive
strength using a uniaxial compression testing machine at 1, 7
and 28 days. Three replicates of each age were used for determin-
ing the average and experimental bounds of the data. The Lime-
SCBA samples were then oven dried at 105 °C to prevent further
hydration reactions occurring and the samples milled to a fine
powder (<10 lm) for residual CaO content analysis by XRD to
determine pozzolanic activity of the SCBA.
Normal consistency of the cement-SCBA specimens were deter-
mined using a manual Vicat Apparatus in accordance with
AS2350.3 [48]. The SCBA and the cement were both treated as
cementitious content for the calculation of normal consistence.
The setting times of cement-SCBA were determined using an auto-
matic Vicat Apparatus in accordance with AS2350.4 [49]. The com-
pressive strengths of cement-SCBA pastes were determined based
on the average of 3 specimens at each age (1, 7 and 28 days).
Crushed samples were then oven dried at 105 °C and milled to a
fine powder (<10 lm) in a zirconium and agate mortar for XRD
mineralogy determinations of cement hydration products.
2.4.2. Mortar pozzolanic activity
The pozzolanic activity of the mortars with SCBA replacement,
was determined from the relative strengths of the test mortars
determined at 28 days [10]. One compressive strength determina-
tion consisted of 3 specimens with a test at each end of the prism
resulting in an average strength based on the 6 individual tests as
described in the standard [10]. The pozzolanic index (PI) was then
calculated using Eq. (1).
T 28
ðPIÞ ¼  100 ½10 ð1Þ
C 28
where
T28 = the mean compressive strength of the test mortar at
28 days and,
C28 = the mean compressive strength of the control mortar at
28 days.
2.4.3. Acid resistance in mortars
The acid solution used for mortar tests was a 1% sulphuric acid
solution, which is considered to replicate a sewer environment
[7,53,54]. A liquid to solid ratio of 4:1 was maintained and the
solution was refreshed every 2 weeks. Sulphuric acid resistance
of mortars with SCBA replacing cement was determined qualita-
tively by visual inspection of the mortar cubes before and after acid
exposure. The compressive strengths of mortars exposed to acid for
0, 28 and 90 days were determined based on the average of 3 spec-
imens for each of the 5 mortar mixes. The compressive strengths of
the 5 mixes that had received no acid exposure but were of the
same age were compared with the acid exposed samples to deter-
mine any loss in strength. The cube specimens were weighed
after drying the surfaces with a cloth, after 0, 28 and 90 days acid
290 E. Arif et al. / Construction and Building Materials 128 (2016) 287–297

Table 3
Mortar mix proportions.

Mix Designation GP Cement (g) CEN Standard Sand (g) SCBA (g) Water (g)
MC 450.0 1350.0 0 225.0
M5 427.5 1350.0 22.5 235.0
M10 405.0 1350.0 45.0 243.0
M15 382.5 1350.0 67.5 256.0
M20 360.0 1350.0 90.0 268.0

exposure to determine the extent of any mass loss as a proxy for 100
the acid resistance of the mortars. 90
80

Cumulave passing (%)

3. Results and discussion 70
60
3.1. SCBA and cement characterization
50
The chemical composition of the OPC and the SCBA as deter- 40
mined by XRF, show that the SCBA is high in silica at 78.498%
30
and the OPC has low silica, at 19.189% (Table 4) suggesting that SCBA

the material contains few aluminosilicates. However, the content 20 cement

of SiO2 + Al2O3 + Fe2O3 of the SCBA is 89.618%, which is above the 10

requirement of 70% to classify as a class F pozzolan. The carbon
0
fraction of the SCBA is 7.150% which is slightly higher than the 0.01 0.10 1.00 10.00 100.00 1,000.00
allowable limit of 6.0% for a pozzolan ash in the Australian stan- Parcle Size (μm)
dards [13]. The high carbon content is responsible for the black
color of the ash and is likely a result of uncontrolled combustion Fig. 1. Particle size distributions of SCBA and GP cement.
conditions [18], this high carbon content could be removed mostly
by sieving as it is quite coarse.
SCBA and the OPC particle size distributions show that the SCBA The XRD patterns (Fig. 3) show an extremely strong sharp and
is significantly coarser (Fig. 1). SCBA has only 65% of particles narrow a-quartz peaks (1; Fig. 3) and a broad hump that is charac-
below 50 lm where as the cement had over 85% of particles below teristic of amorphous minerals (5–2 Å, or around 4 d coupled 2-
50 lm. The SCBA was found to have a lower specific gravity at 1.95 theta/theta, wavelength (WL) = 1.78897; Fig. 3). However, the
than the cement at 3.15. This lower specific gravity is broad amorphous hump is very shallow compared to the a-
often reported and is usually in the range of 1.85 to 2.65 quartz response, suggesting that semi-amorphous/amorphous
[24,29,38,39,55]. (reactive-mineral) fraction is relatively small.
SEM imaging show that the majority of particles are irregularly Data from the XRD and SEM analyses of the ash, and indicated
shaped, porous with only a minor numbers of spherical particles operating temperatures of the mill, suggest that the silica in the
(Fig. 2). The four marked particles in Fig. 2b were selected for ash is being transformed through a series of polymorphs and par-
EDS elemental identification (Table 5) and indicate that particles tially melted. At low pressures (typical of boilers) silica poly-
1, 2 and 4 are mostly silica, but do have some aluminium present morphs form 3 groups (Table 6) each with 2 closely related
suggesting Al substitution for Si in the system. Particle 3 was found members; a low-temperature member given a prefix a-, and a
to have a higher aluminium:silica ratio but with potassium and high-temperature member with a b-prefix. Despite this only
iron also present and is probably an aluminosilicate with minor a-quartz is stable at normal ambient conditions and all other silica
hematite. Particle 4 appears to have molten, which in combination polymorphs transform into a-quartz given sufficient time.
with the EDS results, indicate that it may be an amorphous silicate. Although other silica polymorphs (Table 6) are meta-stable under
It has been reported elsewhere that spherical ash particles are gen- different conditions, these conditions are mostly at high tempera-
erally aluminosilicates whereas prismatic particles are silica ture, some may occur at low temperatures and pressures under
whereas fibrous particles are carbon [56,57], but the data here sug- conditions where quartz is stable (Table 6). Generally, at normal
gest that silica has melted. atmospheric pressure a-quartz transforms at 573 °C into
b-quartz, and upon further heating to 870 °C into b-tridymite and
then to b-cristobalite at 1470 °C; at 1705 °C b-cristobalite finally
Table 4 melts.
Chemical composition of SCBA and GP cement used in this study as determined by
XRF. 573  C ! 870  C ! 1470  C ! 1705  C ! Silica
aQuartz bQuartz bTridymite bCristobalite Melt
%wt SCBA GP Portland Cement
SiO2 78.498 19.189 However, b-quartz does not usually transform to b-tridymite
Al2O3 7.273 3.489 unless it is somewhat impure [58], and often the b-quartz-
Fe2O3 3.847 2.490 tridymite transition is skipped and the sequence looks like this:
CaO 1.280 58.161
MgO 1.281 0.770 573  C ! 1050  C ! 1705  C ! Silica
SO3 1.553 4.343 aQuartz bQuartz bCristobalite Melt
Na2O 0.697 <0.001
K2O 1.414 0.331 As long as the temperature changes are slow, the above process
COH 1.328 10.498 is fully reversible, however greater complexity is generated when
LECO Carbon 7.150 0.670 the temperature is increased or decreased rapidly. For example
LECO Nitrogen 0.090 0.030
very rapid heating of quartz shows that it will still undergo a phase
 E. Arif et al. / Construction and Building Materials 128 (2016) 287–297 291

Similarly, if a silica melt is cooled quickly, it will avoid phases

and its disordered liquid structure will be preserved as a super
cooled liquid or an amorphous silica glass; lechatelierite when
found in nature. However, the XRD pattern (Fig. 3) indicates that
the majority of the silica is present as a-quartz, rather than the
often reported a-cristobalite for bagasse derived silica [18,59],
which coupled with the melting effects observed in some phy-
toliths (Fig. 2), indicate that the bagasse rapidly introduced to
and burnt at temperatures exceeding 1550 °C and that cooling
to about 870 °C but relatively slow below this to preserve the a-
quartz, and low level of semi-amorphous silica.

3.2. Pozzolanic activity

3.2.1. Pozzolanic activity of SCBA with lime

The pozzolanic reaction occurs when reactive aluminosilicates
interact with Ca(OH)2 (portlandite) in the presence of water and
form calcium silicate hydrates (CSH). XRD analysis has therefore
been used to track the consumption of Ca(OH)2 in potential poz-
zolan systems [26,50]. In a similar study [26] lime-SCBA pastes
showed an absence of the Ca(OH)2 peak at 28 days, suggesting
the SCBA used was a probable pozzolan. The XRD patterns in
Fig. 4 show there is still abundant portlandite in the 28 day
hydrated pastes. The slight reduction could be from limited poz-
zolanic reaction occurring. The limited pozzolanic reaction evident,
is most likely from the reduced silica activity from the transition
from a-cristobalite to a-quartz, and an almost absence of semi-
amorphous silica (Figs. 2 and 3; Table 6). Hence, it is highly likely
that bagasse ash from high efficiency boilers of co-generation
plants may act more as a filler than a pozzolanic material.
Compressive strength development of lime-SCBA pastes at 7
and 28 days (Fig. 5) show that compressive strengths increase from
7-day strength by about 150% at 28 days; 1 day data were not cal-
culable due to the paste being too wet for testing. This increase
may be due to some pozzolanic activity of the SCBA, however the
strengths are minimal (<10 MPa) and in combination with the
low amorphous silica (Fig. 3), suggest that the lime paste harden-
ing may well be because of lime carbonation [26], although no sig-
nificant CaCO3 was identified in the XRD scan.

3.2.2. Pozzolanic activity of SCBA in cement pastes

Pozzolan reactions occur at a slower rate than the cement
hydration reactions [50]. Therefore, in a blended cement there
would be an initial increase in portlandite (Ca(OH)2) content from
cement hydration followed by portlandite decreases due to poz-
zolan consumption. The XRD patterns of the cement pastes, with
increasing amounts of SCBA at all ages (Figs. 6–8) show decreasing
Fig. 2. SEM images of SCBA at (a) 270 magnification and (b) at 1750 portlandite concentrations, except for the 5% SCBA-cement paste
magnification. Particle 1: Irregular and porous silica, Particle 2: Incomplete
where a slight increase over the control paste for 1- and 7-days
combustion showing cell structure (bright white lines in particle) and mostly
crystalline silica, Particle 3: Irregular silica with minor amounts of hematite and
curing is seen (Figs. 6–8). The portlandite reduction for SCBA con-
Particle 4: Spherical molten amorphous silica. tent above 5% are most likely from a diluent effect that reduces the
extent of the cement hydration reaction, which is most likely
linked to the to a-quartz content (Fig. 3) and reduced pozzolanic
Table 5 activity of the ash. The diluent effect is also observable by the
Qualitative elemental identification of particles in SCBA by energy dispersive
increasing a-quartz peak as the SCBA content is increased
spectroscopy.
(Fig. 7). Furthermore, there is an increased portlandite content
Particle ID Morphology EDS Elemental Identification as Oxides for all cement paste mixes at 28-days from the 1- and 7-day curing
Major oxides times, which also suggests that little or no pozzolanic reaction is
+1 Irregular/Porous SiO2, Al2O3 occurring. However, at 5% SCBA additions to the cement paste a
+2 Tubular/Prismatic SiO2, Al2O3 5.9% increase in portlandite is seen, whereas the other 4 mixes
+3 Irregular SiO2, K2O, Fe2O3, Al2O3 all had increases in portlandite in excess of 11%. These portlandite
+4 Spherical SiO2, Al2O3
changes would tend to imply that in small quantities (5%) the SCBA
has beneficial properties to cement hydration, but at higher con-
transition to b-quartz, but the b-quartz will then ‘‘skip” the b- centrations the diluent effect outweighs the beneficial properties.
cristobalite transition directly melting at a much lower tempera- Compressive strength development in the cement-SCBA pastes
ture of 1550 °C. (Fig. 9) reveals that the 1-day strength development of all pastes
292 E. Arif et al. / Construction and Building Materials 128 (2016) 287–297

Fig. 3. XRD patterns of SCBA showing quartz silica peaks (1) and calcium aluminium silicate (2).

Table 6 8
Low pressure polymorphs of silica [58].
Compressive strength: Mpa

7
High- or b-polymorph b-Quartz b-Tridymite b-Cristobalite
6
Stable at 573–870 °C 573–870 °C >1470 °C
Metastable at – 117–870 °C 270–1470 °C 5

Low- or a-polymorph a-Quartz a-Tridymite a-Cristobalite 4

Stable at <573°C – – 3
Metastable at – <117 °C <270 °C
2
1
0
7 28
Age: Days

Fig. 5. Compressive strength development of lime and SCBA pastes at 7 and

28 days.

3.2.3. Pozzolanic reactivity of SCBA in mortars

Fig. 4. XRD patterns at wavelength (WL) 1.78897 Å, of the lime-SCBA pastes at 1, 7
and 28 days showing the portlandite (Ca(OH)2) peak.
containing SCBA is reduced. The data also reveal that increasing
SCBA concentration reduces the strength progressively as seen by
the 20% SCBA showing the greatest loss in strength with a reduc-
tion of over 72% at 1 day. However, at a 5% cement replacement
level (CRL) at both 7- and 28-days have 9.6% and 4.6% strength
increases respectively. At 7- and 28-days curing CRL greater than
5% resulted in reduced strengths (Fig. 9). Despite this, cement
pastes at 10% CRL show strengths at age 7- and 28-days curing that
are comparable to the control strengths, with over 90% of the con-
trol cement paste strength (Fig. 9). These strength results are in
agreement with the XRD analysis of the same pastes (Figs. 6–8),
which show that there may be limited pozzolanic reaction occur-
ring at 5% CRL. The limited reactivity of the silica is due to the
phase transitions induced by very high burn temperatures of the
co-generation plant.
The pozzolanic indices (Eq. (1)) of SCBA mortars (Table 7) indi-
cate a decrease in pozzolanic index with increasing SCBA content,
and are commensurate with other data presented. The minimum
pozzolanic index (PI) or relative strength required to classify a
material as a pozzolan is 75% [13]. The results here indicate that
the M20 sample with a PI of 72% falls below the required relative
strength. This would appear to indicate that the SCBA contribution
to strength development is more likely due to a pore filler effect
rather than pozzolanic reactions and is commensurate with other
observations. However, it should be noted as the SCBA content
increases so does the water/binder ratio, and it is widely accepted
that an increase in water results in reduced strength and durability
[3]. As such, this would seem to imply that the SCBA content alone
does not correlate to the strength loss, rather, the relative strength
test results (Table 7) suggest that whilst the SCBA has a limited
pozzolanic activity it may also benefit mortar and concrete through
the pore filler effect [29].
3.3. Influence of SCBA on the fresh properties of cement
3.3.1. Water demand
Water demand in cement pastes and mortars increased as SCBA
replacing cement levels increased and the normal consistency also
 E. Arif et al. / Construction and Building Materials 128 (2016) 287–297 293

Fig. 6. XRD patterns at wavelength (WL) 1.78897 Å, of cement-SCBA pastes at 1 day showing peaks of (1) quartz; (2) calcium silicate; and (3) portlandite.

Fig. 7. XRD patterns at wavelength (WL) 1.78897 Å, of cement and SCBA pastes at 7 days showing peaks of (1) quartz; (2) calcium silicate; and (3) portlandite.

Fig. 8. XRD patterns at wavelength (WL) 1.78897 Å, of cement and SCBA pastes at 28 days showing peaks of (1) quartz; (2) calcium silicate; and (3) portlandite.
294 E. Arif et al. / Construction and Building Materials 128 (2016) 287–297

90 Table 8
CP0A
Flows and relative water requirements of mortar with 0, 5, 10, 15 & 20% SCBA
80 CP5A
replacing cement.
CP10A
CP15A
70 Mortar Mix Flow% Relative water requirement%
Compressive Strength: MPa

CP20A
60 Control 107 100
M5 108 104
50 M10 108 108
M15 105 114
40 M20 109 119

30

20
Table 9
10 Setting times of cement with 0, 5, 10, 15 & 20% SCBA replacing cement (by mass).

Mix ID Initial Setting Time (min) Final Setting Time (min)

0
Day 1 Day 7 Day 28 CPA0 122 207
CPA5 139 283
Fig. 9. Compressive strengths of Cement pastes with 0, 5, 10, 15, and 20% SCBA CPA10 152 293
replacing OPC at 1, 7, and 28 days. CPA15 180 318
CPA20 194 325
AS3972 limits P45 6600
Table 7
Pozzolanic index and compressive strengths of test mortars with SCBA replacing OPC
at 0, 5, 10, 15 & 20% (wt).
ever, this is not inhibitory to SCBA utilization in mortars and con-
Mix ID SCBA content (wt%) 28 day Strength (MPa) Pozzolanic Index (%) cretes, as the addition of chemical water reducers and
MC 0 57.7 100 superplasticisers are often employed to compensate for an
M5 5 56.2 97 increased water demand whilst achieving the desired workability
M10 10 50.3 87
and consistency of the fresh cement [38].
M15 15 50.3 87
M20 20 41.3 72

3.3.2. Setting times

increased; the control cement paste (CP0A) was 29.5% (Fig. 10). The
test cement pastes all showed an increase from this by 12.9%,
25.8%, 34.2% and 44.1% for CP5A, CP10A, CP15A, and CP20A respec-
tively (Fig. 10). This trend is reflected in the W/B ratio needed to
achieve standard flows in the test mortars (Table 8). The increase
in water demand is most likely due to the porous nature of the par-
ticles increasing the water absorption of the mix [39]. Also the pre-
dominance of irregular shaped particles of the SCBA is likely to
increase friction, reducing workability thus increasing water
demand [27]. Hence, because the SCBA is both porous and angular
the increased water consumption is readily explainable by these
two factors. However, compounding this is that the specific gravity
of SCBA is substantially less than cement; lower density results in a
greater total volume of material in the paste. As the replacement of
cement was calculated on weight, then a greater volume of mate-
rial requires lubrication and the water content must increase to
compensate and contributes to the increased water demand. How-
45
40
Normal Consistency (%)
The setting times of cement pastes of normal consistency, con-
taining increasing amounts of SCBA are listed in Table 8. There was
an increase in both the initial and final setting times. The increase
in the setting times may be due to the reduction in cement content
and from increases in water as SCBA content increases (Table 7).
Increases in setting times have previously been reported using
SCBA [43], however all setting times were within the limits set
forth in AS3972 [45] where the initial setting time should be
P45 min and the final setting time should be less than 10 h
(Table 9).
3.4. Effect of SCBA on the sulphuric acid resistance of mortars
incorporating SCBA
3.4.1. Compressive strength of acid exposed mortars
The compressive strengths of both the mortars exposed to 1%
sulphuric acid solution for 28 days after an initial 7 days lime
water curing and the mortars cured for 35 days in the moist curing
environment are compared in Fig. 11. The compressive strength of
mortars exposed to acid decreases for all mixes except M20. The
greatest loss in strength is by the control mortar with an average
loss of over 57%. There is a slight increase in strength of the M20
acid exposed mortar compared to the lime water cured M20 but

is not statistically significant. For the 28-day acid exposed mortars

35 the greatest strength is achieved by M10, where there seems to be
a synergy of improved acid resistance at 20% addition of SCBA on
the one hand, and improved strength at only 5% addition of SCBA
30 on the other. This synergy results in all additions of SCBA having
similar strengths at 28 days acid exposure.
25 The compressive strengths of both the mortars exposed to 1%
sulphuric acid solution for 90 days after an initial 7 days lime
water curing and the mortars cured in standard moist curing for
20 97 days are also shown in Fig. 11. It shows that as the length of
0 5 10 15 20 25
exposure to the acid solution is extended the compressive strength
SCBA replacing OPC % (wt)
of all the mortar mixes decrease to a greater extent. At 90 days
Fig. 10. Normal consistency of cement pastes with 0, 5, 10, 15, and 20% SCBA however the acid resistance of the M20 blend seems to have pro-
replacing OPC by weight. vided this mortar with the greatest protection from strength loss.
 E. Arif et al. / Construction and Building Materials 128 (2016) 287–297 295

80

70

60

Compressive Strength: MPa

50

40

30

20

10

0
35 days curing 28 days acid exposure + 7 97 days curing 90 days acid exposure + 7
days curing days curing
MC M5 M10 M15 M20

Fig. 11. Compressive strength of 50 mm mortar cubes with increasing SCBA for mortars with 35 days of standard moist curing conditions; 28 days 1% H2SO4 exposure in
addition to 7 days standard moist curing; 97 days in standard moist curing conditions; and for 90 days 1% H2SO4 exposure after initial 7 days curing.

The control mortar shows an average loss of over 79% whereas the
M20 mix has an average loss of about 60% and also achieves the
greatest compressive strength in the 90 day acid exposed mortars.
These results indicate that SCBA has a capacity to either neutralise
acid and thus improve the acid resistance of concretes and mortars
or possibly that the SCBA exerts a pore refining effect thus reducing
the permeability of the acidic solution into the cement matrix
[60,4]. In other research it has also been reported that SCBA
improved the acid resistance of cements [43] most likely due to
reduced permeability.
3.4.2. Mass loss of acid exposed mortars and qualitative evaluation
Mass changes of mortars exposed to acid for 28 and 90 days and
unexposed samples of the same age are compared (Fig. 12). Fig. 12
shows that as SCBA content increased the mass loss of mortars
exposed to 1% H2SO4 for 28 and 90 days decreased, similar obser-
vations have been made previously [43] and also with other waste
SCM materials; rice husk ash, coal fly ash [60] and even non poz-
zolanic materials such as neutralised bauxite refinery residue
290
280
270
Weight (grams)
[54]. Also the visual evaluation of the mortars (Fig. 13) show that
the mortars with 20% SCBA replacing cement have minimal surface
degradation at 90 days (Fig. 13c), whereas the control mortar is
noticeably eroded as early as 28 days acid exposure (Fig. 13b). At
90 days acid exposure the M20 is still intact at the surface with
minimal degradation whereas the MC at 90 days is considerably
degraded (Fig. 14). The improved resistance may be due to the for-
mation of a buffer zone at the surface of the mortar which is pre-
venting the detrimental formation of the expansive ettringite and
gypsum [54] or may be due to pore refinement reducing the rate
of deterioration [61]. Ettringite, the cause of much of the mass
wasting and spalling of concretes and mortars in sulphate-rich
environments [54], may well be reduced by a shift in the cement
composition from C3A, towards a C2S-rich mineralogy, reducing
aluminium availability. Closer examination of the XRD patterns
(Figs. 6–8), does not provide sufficient detail to confirm this,
because of the over whelming portlandite peak at 2.63 Å, although
there is a noticeable shoulder to the quartz peak that appears to
develop with increasing SCBA additions and curing time, which
may be an unresolved silicate phase (Figs. 6–8). However, this
requires further investigations outside the scope of this paper to
resolve the issue and determine the real factors behind the signif-
icantly reduced spalling and mass loss, particularly when there is
such a significant drop in compressive strength (Fig. 11).

260 4. Conclusions
0 days acid
exposure
250 28 days acid The SCBA as received from a high-efficiency co-generation boi-
exposure
90 days acid
ler does not contain significant amorphous silica, but contains
240 exposure crystalline a-quartz. Consequently, it appears the combustion tem-
perature within the high-efficiency co-generation boiler has con-
230 verted the silica from previously reported a-cristobalite in
bagasse [18,59] to a-quartz [58] substantially reducing the poz-
220
MC M5 M10 M15 M20
zolanic reactivity in cement and lime pastes. XRD data of both
Mortar Mixes the lime-SCBA and cement-SCBA pastes show little or no poz-
zolanic activity is occurring, except when used in cement pastes
Fig. 12. Comparison of the average weights of mortars with 0, 5, 10, 15 & 20% SCBA at 5% replacement. Similarly, compressive strength testing of the
replacing cement by weight at 0, 28 and 90 days acid exposure at ages 7, 35 and
cement pastes also suggests that at 5% cement replacement level,
97 days respectively.
the SCBA is potentially pozzolanic. However, despite this mortars
296 E. Arif et al. / Construction and Building Materials 128 (2016) 287–297
Fig. 13. Mortars with SCBA replacing cement at 0, 5, 10, 15 & 20% by mass exposed to 1% sulphuric acid solution for (a) zero days, (b) 28 days and (c) 90 days.
Fig. 14. Comparison of MC mortar with 0% SCBA, and M20 with 20% SCBA replacing
cement (wt%) at 90 days exposure to 1% sulphuric acid solution.
with up to 15% SCBA replacing cement achieve a pozzolanic index
above 75%, which suggests increases in pozzolanic activity by the
relative strength tests are more likely a result of the filler effect
[29]. Hence, the addition of high-efficiency Co-Generation Boiler
SCBA’s into cement systems leads to increased consistencies, water
demand [27], and setting times [43]. The pozzolanic tests con-
ducted in this study were performed to the Australian standards
where water is increased to maintain workability. It is recom-
mended that future studies of the pozzolanic activity of SCBA vary
superplasticizer content rather than water. Despite the apparent
lack of pozzolanic activity high-efficiency co-generation boiler
SCBA’s improved sulphuric acid resistance at all replacement
levels, which may be due to filler effect reducing acid permeability
into the cement matrix [43], and/or by slight shifts in chemistry to
more silica bearing phases through the limited pozzolanic reac-
tions [62]. It is recommended in future studies on filler potential
of SCBA that water absorption, mercury intrusion porosimetry or
similar studies be conducted. Hence, the high-efficiency co-
generation boiler SCBA used in this study may be used in mortars
as a cement substitute cement up to 15%, but further studies using
the SCBA as a filler rather than a SCM would provide important
insights into high-efficiency co-generation boiler SCBA utilization.
Acknowledgements
The authors are grateful for the support provided by Sugar
Research Australia (SRA; formally SRDC, Sugar Research develop-
ment Corporation) via the grant SRDC SCU03. Financial support
was also provided by Australian Biorefining Pty Ltd (Adam Blunn)
as an industry partner to the grant SRDC SCU03. Many thanks are
extended to the staff and students at the School of Environment
Science and Engineering, Southern Cross University, who assisted
in the laboratory work for data collection.
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