Journal of Cleaner Production 316 (2021) 128242

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Journal of Cleaner Production

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

Influence of different processing methods on the recycling potential of

agro-waste ashes for sustainable cement production: A review
R. Rithuparna, V. Jittin, A. Bahurudeen *
Department of Civil Engineering, Birla Institute of Technology and Science Pilani, Hyderabad Campus, Hyderabad, India

A R T I C L E I N F O A B S T R A C T

Handling editor. Prof. Jiri Jaromir Klemeš The improper disposal method of the agro-waste and currently followed practice of carbon-intensive open-field
burning causes severe environmental pollution. Hence, it is essential to identify efficient ways of utilising these
Keywords: agro-residues. However, the absence of proper understanding of their characterisation and processing method
Agro-waste ash hinders the acceptance of the agro-residual ashes in the cement industry. Although the pozzolanic performance
Blended cement
of several agro-waste ashes is evidently reported in the earlier studies, a comprehensive review of the processing
Burning
methods to be adopted for different agro-waste ashes is highly limited. Hence, the present review mainly focuses
Grinding
Processing on the influence of different processing methods such as grinding, burning, chemical, thermomechanical and
Thermomechanical thermochemical on the pozzolanic performance of agro-waste ashes. The effect of different processing methods
on physical, chemical, and mineralogical characteristics of agro-waste ashes such as rice husk ash, sugarcane
bagasse ash, palm oil fuel ash, wheat straw ash, corn cob ash, corn stalk ash, rice straw ash, bamboo leaf ash,
maize stalk leaf ash and elephant grass ash is presented. Moreover, variations in the fresh and hardened prop­
erties of concrete blended with the treated agro-waste ashes are discussed. It is observed from the review that the
grinding of agro-waste ashes increases their pozzolanic activity index above 75%, and subsequently, 10–50%
enhancement in the compressive strength is reported. Thermal processing improved the pozzolanic performance
by decreasing the loss on ignition, and the optimum burning temperature of agro-waste ashes range from 500 to
700 ◦ C. Furthermore, chemical treatment increased the specific surface area and decreased the loss on ignition of
agro-waste ashes, thereby enhanced the strength and durability of blended cementitious systems. Moreover,
synergistic use of processing methods is found to be efficient than respective individual processing methods.
Based on a detailed review, it can be stated that the optimum conditions of processing to be adopted are diverse
for different agro-wastes. The current study also presents the optimum parameters for the processing of different
materials based on the extensive review. Therefore, by adopting an appropriate method of processing, the agro-
waste ashes can be effectively utilised as supplementary cementitious materials.

1. Introduction
The global production of crop residues has been progressively
increasing over the past few decades, and the production is estimated at
280 Mt/year for cereal crops and 3758 Mt/year for 27 food crops (Lal,
2005). The residues produced after harvesting and processing of the
crops include stalks (maize), straws (rice, wheat, sugarcane), leaves,
husk (rice, wheat), seed shells (palm) etc. The disposal of agricultural
wastes is a rising environmental concern in most countries. The
commonly practised methods are dumping the wastes in barren land and
burning the agro-wastes in an open field by farmers, leading to severe
land and air pollution. In Asia, the burning of crop residues in the field
comprises 34% of the total biomass burnt in a typical year. Considering
the case of agriculture-based economies like China and India, open-field
burning of residues contribute to a significant amount of greenhouse gas
emission (Streets et al., 2003). Hence, it is of great importance to find
more viable and environment-friendly solutions for agro-waste disposal.
Some of the applications of these wastes are their utilisation as biomass
fuels which can be a replacement for conventional coal. In addition to
the use of agro-waste as biomass, there are various applications of
agro-wastes. They can be utilised as bio-fertilisers that can be an alter­
native to hazardous chemical fertilisers. Another application of
silica-rich agro-waste materials is to extract the silica from the materials
and use it in Li-ion battery anodes (Sharma et al., 2020). Rice husk was

* Corresponding author. Department of Civil Engineering, Birla Institute of Technology and Science Pilani, Hyderabad Campus, Hyderabad, 500078, India.
E-mail address: bahur@hyderabad.bits-pilani.ac.in (A. Bahurudeen).

https://doi.org/10.1016/j.jclepro.2021.128242
Received 8 November 2020; Received in revised form 5 June 2021; Accepted 5 July 2021
Available online 7 July 2021
0959-6526/© 2021 Elsevier Ltd. All rights reserved.
R. Rithuparna et al.
used as an additive in many applications such as refractory brick pro­
duction, flame retardants and particle wood cardboards, etc. (Jeetah
et al., 2015; Phonphuak and Chindaprasirt, 2015). Sugarcane bagasse, a
fibrous residue obtained from sugarcane after extracting sugarcane
juice, is also reported to have several applications. Thermochemical
conversion of sugarcane bagasse yields hydrogen and bio-oil. In addi­
tion, ethanol can be produced as a by-product of sugarcane processing.
Bagasse is also widely used in paper production (Gopinath et al., 2018).
Furthermore, sugarcane straw can be used as a feed to produce
bio-energy, bio-fuels, composites, and adsorbent (Aguiar et al., 2021;
Menandro et al., 2012). Corn cob finds use as a potential raw material in
industrial biotechnology processes (Pérez-Rodríguez et al., 2016).
Wheat straw is known for several applications such as raw material for
animal bedding, in insulation board, as loose-fill insulation, in com­
posites, as heating fuels, in bio-refineries, in bio-plastics, as source ma­
terial in pulp industry, in production of paper, as a solid state for
microbial growth and as an absorbent of uranium residues (Canizares
et al., 2020).
Even though the agro-wastes have found different applications in
various industries, the disposal problem of agro-waste residual ashes
generated as secondary by-products in these industries persist. Similar to
the utilisation of agro-waste, the residual agro-waste ashes (AWA) also
find various applications in different industries. Agro-waste ashes
consist of a high amount of silica and can be used to synthesize glass and
glass-based ceramics (Danewalia et al., 2016). Rice husk ash (RHA) was
reported to be used as an absorbent, catalyst, abrasive agent, oil
adsorbent, sweeping component fertilizer and a suspension agent for
porcelain enamels, in addition to its application in the construction
sector (Moayedi et al., 2019; Mor et al., 2016; Singh, 2018). Another
application of rice husk ash is its use as an insulation powder in steel
casting tundish (Kim et al., 2017). Sugarcane bagasse ash (SCBA) can be
used in the rubber industry as a replacement for commercial silica
(Torres et al., 2021), as a filter, soil stabilization (James and Pandian,
2017).
These ashes are generally rich in reactive silica and can be a potential
replacement material for cement, with proper processing before their
utilisation. This will not only act as an effective means of waste reuti­
lisation but also paves the way for an additional source of income for the
farmers. The rising demand for cement over the years and the release of
huge quantities of anthropogenic carbon dioxide from the cement in­
dustry dictates the necessity of finding cementitious materials which can
be a substitute for cement. The depleting amount of non-renewable raw
materials such as limestone used for cement manufacturing, is another
reason for the need to explore alternate options. The application of agro-
waste in concrete imparts good mechanical properties. The pozzolanic
materials contribute to the strength of concrete in two ways, firstly due
to the filler effect and secondly owing to the pozzolanic reactivity.
However, long-term properties of control concrete were found to be
better than agro-waste based concrete (Vo and Navard, 2016). The most
widely accepted supplementary cementitious materials (SCM) are in­
dustrial by-products such as fly ash from thermal power plants, slag from
the steel industry and silica fume from the silicon industry. In addition,
several agro-waste residual ashes such as RSA, SCBA, wheat straw ash
(WSA), corn cob ash (CCA), etc. have considerable potential as a cement
replacement material and help to make the cement industry more sus­
tainable (Aprianti et al., 2015). A concrete blended with agro-ashes
obtained after proper processing exhibits comparable or better perfor­
mance than conventional concrete.
RHA and rice straw ash (RSA) are by-products of the rice industry.
Rice husk is the outer cover of rice with low nutritional value. During the
milling of rice, the rice husk is removed. Later rice husk is used as a fuel
in the boiler of the rice processing industry and hence, produces RHA.
RSA is produced due to the combustion of rice straw (Athira et al.,
2021). Sugarcane bagasse, after extraction of juice, is used as feedstock
in the cogeneration boiler to produce SCBA. In addition to bagasse, the
straw residue is also used in boilers to yield SCSA (Gopinath et al.,
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Journal of Cleaner Production 316 (2021) 128242
2018). Palm oil fuel ash (POFA) is a by-product of the palm oil industry.
It is produced due to the combustion of palm fibres and shells in the
boiler after palm oil extraction (Hamada et al., 2018). Wheat is one of
the main agricultural product grown in different parts of the world. The
use of wheat straw in cogeneration boilers produces WSA, silica-rich
biomass ash (Biricik et al., 1999). Calcination of corn cob, a product
obtained during production of corns, produces CCA. Similarly, corn stalk
ash (CSA) is generated as a by-product from the combustion of corn stalk
(Tumba et al., 2018). In countries like Brazil, elephant grass is cultivated
as biomass for cogeneration. The resulting yield on burning elephant
grass is about 4–5% (Nakanishi et al., 2016). The influence of AWAs as
supplementary cementitious materials in concrete was reported in
various literature. The utilisation of untreated AWAs faces significant
challenges owing to high carbon content and the presence of alkali
metals in the residues. The incorporation of most of the raw AWAs was
found to decrease the slump of concrete except for POFA and WSA
blended concrete. Instead of energy-intensive processing methods such
as burning and grinding, a simple sieving process is adequate to obtain
reactive SCBA for use as a pozzolan (Charitha et al., 2021). Researches
on agro-wastes revealed that burning of the residues under controlled
conditions would produce ashes with high reactivity. However, higher
calcination beyond 900 ◦ C has an adverse effect on the reactivity of
RHA, SCBA, and RSA. It was stated that burning of the residues at high
temperature caused the formation of potassium melt which traps the
carbon and volatile matter present in the residues from escaping during
burning (Bie et al., 2015; Krishnarao et al., 2001). Chemical
pre-treatment of the agro-waste residue prior to burning is recom­
mended to leach out the alkali metals which thereby aid in the removal
of carbon (Cordeiro and Kurtis, 2017; Salas et al., 2009; Shakouri et al.,
2020). Most of the researchers suggest an optimum burning temperature
and duration for various agro-wastes. Burning the agro-residues below
the optimum condition will result in the presence of unburnt carbon,
whereas crystallisation of silica occurs when the material is burnt above
the optimum temperature required. For some of the materials such as
RHA and SCBA, grinding the ashes showed enhancement in the pozzo­
lanic reactivity owing to the reduction in particle size and higher specific
surface area. Therefore, it can be stated that depending on the source,
nature of biomass and required level of pozzolanic reactivity, agro-waste
residues need different methods and degrees of processing.
From the earlier research studies, it is observed that different pro­
cessing conditions have a remarkable influence on the pozzolanic per­
formance of agro-waste ashes. Although unprocessed agro-waste ashes
have less pozzolanicity, a simple processing method helps convert them
into highly reactive pozzolans. For instance, Athira et al. stated raw
bagasse ash had lesser pozzolanicity than minimum required pozzola­
nicity index value (75%), and it cannot be directly used in concrete.
However, a simple sieving process increases pozzolanic index value
above 85% and enable its uses as an SCM in concrete. Further grinding of
the sieved bagasse ash to the cement fineness led to 106% of pozzola­
nicity index value, signifying superior pozzolanicity of bagasse ash
(Gopinath et al., 2018). It is evident that a very less reactive pozzolan
can be converted as reactive pozzolan by using the appropriate pro­
cessing method. Hence, it is essential to have an in-depth understanding
of changes in properties of AWAs with respect to different processing
conditions. However, a systematic review specifically on the influence of
different processing conditions for a wide range of agro-waste residual
ashes is highly limited. Hence, the present review primarily focuses on
the influence of various processing methods such as mechanical, thermal
and chemical. Furthermore, the current review provides a scientific
insight into synergistic processing methods such as thermomechanical
and thermochemical treatments in addition to the individual processing
methods, which are not extensively reviewed for agro-waste ashes. The
method of treatment to be adopted is highly governed by the source
variability and level of pozzolanic reactivity of the unprocessed
agro-waste ashes. It is also imperative to consider the level of pozzolanic
reactivity required for the intended application of AWAs blended
R. Rithuparna et al.
concrete. Lack of knowledge on the processing methods to be followed
for potential materials such as POFA, CCA, WSA, RSA, maize stalk leaf
ash, bamboo leaf ash (BLA) etc., hinders their acceptance as a pozzolanic
material in the cement industry. Hence, a thorough review including
different processing methods needs to be adopted for various agro-waste
ashes to encourage their effective utilisation as a cement replacement
material in concrete. For that reason, the present review is mainly
emphasized on physical, chemical, pozzolanic characteristics of the
treated agro-waste ashes. Furthermore, a detailed discussion on the
fresh and hardened properties of concrete blended with treated
agro-waste ashes is presented. Moreover, the current study recommends
the optimum parameters of individual and synergistic processing
methods for a wide range of agro-waste ashes, which aid to choose an
appropriate processing method. In the later part of the paper, a
comparative study on the processing methods adopted for various
agro-waste ashes is illustrated, and recommendations for future research
are also suggested.
2. Methodology adopted for the review
The primary objective is to provide a comprehensive review of the
influence of various processing techniques on the pozzolanic perfor­
mance of agriculture residual ashes. The following research questions
were attempted to be addressed in the present study:
(i) What are the pre-treatment methods adopted for various agri­
culture residual ashes and their influence on the quality of ashes?
(ii) What are the mechanisms involved in the several processing
methods on the performance of agro-waste residual ashes?
(iii) How does the degree of processing affect the quality of ashes?
(iv) How does the prior treatment of agricultural residues influence
the performance of agro-based ash blended concrete in the aspect
of fresh and hardened properties?
(v) Are the conventional techniques of grinding and heat treatment
sufficient for producing good quality ash?
(vi) Can processing be considered effective in enhancing the uti­
lisation of various agricultural by-products as supplementary
cementitious materials?
(vii) Is the combined method of mechanical and thermal treatment
beneficial for enhancing the pozzolanic characteristics of the
agro-based ashes?
A systematic screening of the literature was adopted for collecting
the research articles which are relevant to the present study. Scopus,
Google Scholar, Science Direct and other important databases were used
for obtaining reliable publications. All the journal articles, including
review articles and conference papers, were collected for the study. To
guarantee the quality of the review, only peer-reviewed articles were
considered during the screening process. The entire process of literature
collection was restricted to the fields of environmental science, material
science and engineering and can be divided into several stages. Stage 1
involves search using the keywords such as ‘concrete’, ‘cement’, ‘sup­
plementary cementitious materials’ and ‘agriculture residual ashes’ in
the databases as mentioned above. The second stage of articles collec­
tion was carried out using material specific keywords, namely ‘rice husk
ash’, ‘sugarcane bagasse ash’, ‘corn cob ash’, ‘corn stalk ash’, ‘rice straw
ash’, ‘wheat straw ash’, etc. Taking the aforementioned keywords into
account, 1239 research papers were extracted and from which the list
was further narrowed down to 455 papers using the keywords related to
the processing methods adopted for different materials. A judiciously
planned screening process was followed to reduce the sample size and
avoid articles that are not relevant to the present review. The final
shortlisting was carried out by skimming through the abstract and
conclusion presented, and the articles which were not related to the
focus of this study were omitted. A few articles which answered the
research questions were obtained through the application of
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Journal of Cleaner Production 316 (2021) 128242
snowballing technique as well. Finally, the total count of the articles
which was related to the study setting and research focus was 135. The
articles were further segregated into different categories based on the
method of pre-treatment adopted and the materials under study. From
the literature survey, it can be observed that the processing studies on
rice husk ash and sugarcane bagasse ash dominated the research studies.
Only limited studies were conducted for other agricultural by-products
such as rice straw ash, corn cob ash, wheat straw ash, etc. Qualitative
and quantitative data based on the aim of the research were extracted
from the collected publications. A thorough and in-depth analysis of the
information collected was performed in the present review.
3. Mechanical processing
3.1. Influence of grinding time on particle size distribution and specific
surface area
The residual ashes obtained after burning of agro-wastes usually
have a large particle size and low specific surface area (SSA), which
indirectly affects the pozzolanic activity of the material. Mechanical
processing methods, such as sieving and grinding, have a considerable
impact on the particle size and SSA of these materials. The main ad­
vantages of grinding ashes to high fineness is the possibility of obtaining
finer particles that will fill in the voids of the paste and also enhance the
pozzolanic reactivity of the material (Kroehong et al., 2011). The gen­
eral trend for mean particle size (D50) that can be depicted from Fig. 1
(a) is that D50 is found to reduce considerably at the initial stage as the
grinding time was increased. However, not much change was observed
beyond the optimum grinding time. The difficulty of grinding finer
particles is associated with the high strength and tendency of the par­
ticles to agglomerate, which necessitates higher grinding energy (Cor­
deiro et al., 2009a; Venkatanarayanan and Rangaraju, 2015; Xu et al.,
2015). Cordeiro et al. reported a grinding time of 120 min as optimum
for breaking down all the coarse grains present in the as-received sam­
ples of RHA (Cordeiro et al., 2009a). For palm oil fuel ash (POFA)
samples as well, there was a noticeable decrease in D50 up to 7 h of
grinding, after which the change in particle size was minimal (Ismail
et al., 2010). In a similar manner, the particle size of POFA was reduced
from 119.9 μm to 1.6 μm when the raw POFA was ground for 100 min
(Asrah et al., 2015). On comparing unground POFA (large particles of
size 183 μm) and ground POFA (small particles of size 7.4 μm) samples, a
90% reduction in size was observed owing to the crushing of porous
POFA particles into a smaller size when the ashes were subjected to the
grinding process (Jaturapitakkul et al., 2007).
Cordeiro et al. studied the effect of grinding SCBA in a vibratory mill
and a tumbling mill for different durations. The particle size (D80) of
unground SCBA was 199 μm and the size reduced from 113.2 μm to 34.5
μm after the grinding of SCBA for 30 min–480 min in the tumbling mill.
A higher reduction in particle size from 73.4 μm to 5.4 μm was observed
when the SCBA was ground in the vibratory mill for 8 min to 240 min. It
was reported that after 240 min of grinding, SCBA had some coarse
quartz particles, whereas the cellular structure in SCBA was completely
broken down (Cordeiro et al., 2009c). In the same way, the breaking
down of irregular large particles and cellular structures in raw SCBA to
fine particles as a result of the grinding of SCBA was also stated by
Mohan et al. The particle size was found to reduce from 40 μm to 10.95
μm, when the SCBA was ground for a duration of 120 min, beyond which
the reduction in the particle size was found to be minimal. The ground
SCBA particles were finer than the average size of 53 grade OPC parti­
cles, and hence the filler ability of fine ground SCBA can contribute to
the strength of blended concrete (Mohan et al., 2021). A comparison
between SCBA ground in the two mills showed that significantly finer
particles were formed in the vibratory mill compared to the tumbling
mill after grinding SCBA for the same duration, which indicates that
faster breakdown of particles was attained in the former grinding
method (Cordeiro et al., 2009c). The larger specific surface area of SCBA
R. Rithuparna et al.
Fig. 1. Variation in (a) mean particle size and (b) specific surface area with respect to grinding time.
ground in the vibratory mill (Cordeiro et al., 2008) compared to the
tumbling mill can be clearly observed in Fig. 1 (b). SEM micrographs of
sugarcane straw ash (SCSA) before and after grinding for 50 min showed
that the large irregular particles present in unground SCSA were broken
down into finer particles with a mean diameter of 10.85 μm. The finer
particle size also reflects in the high pozzolanic reactivity of ground
SCSA (Moraes et al., 2015).
Blaine’s air permeability method and Brunauer-Emmett-Teller (BET)
adsorption method are the widely used methods for measuring the
specific surface area of SCMs. From Fig. 1 (b), it can be noted that except
for the RHA used in the study by Xu et al. and Rego et al., SSA was found
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Journal of Cleaner Production 316 (2021) 128242
to be increased as the duration of grinding was increased (Rêgo et al.,
2015). An increase in BET surface area from 2.76 to 11.91 m2/g for
grinding RHA up to 60 min was observed, and thereafter the SSA tends
to decrease due to agglomeration of fine particles (Xu et al., 2015). The
lower SSA reported by Bahri et al. after 16 h of grinding of RHA is
attributed to the collapse of the cellular structure due to excessive
grinding and the subsequent filling of fine particles in the initial pores of
the structure. On the contrary, ground black rice husk ash (BRHA)
produced from incomplete burning of rice husk is less porous compared
to RHA and was found to have higher SSA by 76% compared to un­
ground BRHA (U-BRHA) sample (Bahri et al., 2018). Cordeiro and
R. Rithuparna et al.
Kurtis, studied the properties of SCBA, which was ground for different
durations. The D50 value of ground SCBA was 29.6, 14.7, 6.8 and 4.4 μm
on increasing the grinding time of 8, 30, 120 and 960 min, respectively.
The specific surface area in terms of BET is also increased significantly,
as shown in Fig. 1 (Cordeiro and Kurtis, 2017). Moreover, the specific
surface area of RHA is higher than SCBA for the same grinding duration,
as RHA is highly porous in nature. Grinding of as-received POFA into
three different particle sizes were carried out to evaluate the influence of
particle size on the pozzolanic reactivity of POFA. The Blaine’s fineness
of large particles (34% retained on 45 μm sieve), medium particles
(13.5% retained on 45 μm sieve), and small particles (5% retained on 45
μm sieve) were obtained as 660.5, 719 and 1228.5 m2/kg, respectively
(Jaturapitakkul et al., 2011). Aprianti et al. also reported an increase in
the fineness and specific gravity of POFA after grinding (Aprianti et al.,
2015). Two different milling techniques were employed by Qudoos et al.
to study the pozzolanic efficiency of ground WSA. The WSA sample was
ground using a combination of a ball mill (45 min) and a disintegrator
mill (3 cycles of 5 min each at 32000 rpm), and it had higher SSA
compared to the sample ground in either ball mill or disintegrator mill
alone. The extensive grinding resulted in the availability of inner
amorphous silica, which can be confirmed by the lowering and broad­
ening of crystalline silica peak in the XRD pattern (Qudoos et al., 2020).
In a study by Cordeiro et al., grinding SCBA using vibratory and tum­
bling mills for various durations showed a significant increase in the
fineness of ground particles with a maximum SSA of 1197 m2/kg (6
times higher than unground SCBA) when the SCBA was ground for 240
min in the vibratory mill (Cordeiro et al., 2009c).
3.2. Influence of grinding time on pozzolanic activity
As per ASTM C618, the minimum requirement of pozzolanic activity
index (PAI) is 75% for natural pozzolans (ASTM C618, 2019). Even
though most of the unground AWAs had PAI less than the minimum
Fig. 2. Variation of PAI with respect to grinding duration.
5
Journal of Cleaner Production 316 (2021) 128242
requirement, the values for ground samples were found to be well above
this limit irrespective of the grinding duration, as shown in Fig. 2. The
only exception was the RHA sample studied by Rego et al., which had to
be ground for 300 min to satisfy the requirement (Rêgo et al., 2015). For
instance, even though the PAI of unground SCBA was found to be 50%,
the value was increased to 80% when ground for 480 min in a tumbling
mill and 103% when ground for 240 min in a vibratory mill. Hence, it is
evident that the pozzolanic reactivity of SCBA improves as the specific
surface area increases and particle size decreases due to the grinding
process (Cordeiro et al., 2009c). Similarly, the pozzolanic activity index
was increased from 74% (below ASTM C618 specified limit) to 112.7%
when the as-received SCBA was ground to a finer size of 5.6 μm (Somna
et al., 2012).
The results of the study by Bakar et al. and Ramadhansyah et al.
revealed that there is an optimum grinding time (90 min) for RHA up to
which the PAI increases and after which a noticeable reduction in the
value was observed. This reduction can be attributed to the higher SSA
of the ground samples, which leads to greater water demand to maintain
the same flow and thereby resulting in a decrease in the strength (Bakar
et al., 2011; Ramadhansyah et al., 2012). Some of the researchers re­
ported minimal changes in the PAI of SCBA samples at higher durations
of grinding (Cordeiro et al., 2008; Kameshwar et al., 2020). The
requirement of higher energy for further grinding of finer particles may
be the reason for the small difference in PAI.
The influence of particle size on PAI can be noticed in Fig. 3. It is
evident that the pozzolanic activity of a material is inversely propor­
tional to its particle size and has a direct relationship with Blaine’s
fineness. The smaller the particle size and the larger the SSA, the higher
will be the pozzolanic reactivity of AWAs (Yadav et al., 2020). The ac­
tivity index of SCBA samples was enhanced from 54 to 79% as the
particles were ground to a mean size of 45 μm from 210 μm (Bahurudeen
and Santhanam, 2015). Availability of more number of nucleation sites
for the pozzolanic reaction to take place as a result of higher specific
R. Rithuparna et al.
Fig. 3. Variation of PAI and Blaine’s fineness with respect to mean particle size.
surface area can be one of the reasons for the improvement in pozzolanic
reactivity (Rukzon et al., 2009). Another reason could be the filler effect
of finer particles as it results in better pore refinement and higher
strength of concrete (Cordeiro et al., 2008). The study of pozzolanic
activity using the Chapelle activity method also exhibited similar re­
sults. The amount of lime fixed per gram of pozzolan was found to be
increased from 36 to 298 mg/g on grinding SCBA for 240 min, and 35%
improvement in the Chapelle activity was observed for RHA sample
ground for the same duration (Cordeiro et al, 2008, 2009a). Asrah et al.
studied the effect of particle size on the pozzolanic reactivity of ground
POFA. The highest pozzolanic reactivity among POFA samples with
different particle sizes was for ultrafine POFA (1.6 μm) which is 106%
and then for fine (3 μm) and medium (39.5 μm) sized POFA which are 86
and 81%, respectively (Asrah et al., 2015). Hence, it is evident that the
fineness of AWA particles plays an important role in the pozzolanic
reactivity of the ashes.
3.3. Influence of grinding time on fresh properties of blended cementitious
systems
The higher the slump, the higher will be the workability of the
concrete mixture and the lower will the dosage of superplasticisers (SP)
required for a constant water/binder ratio (w/b ratio). Particle size
distribution and packing density are two parameters which will influ­
ence the water demand and workability of any concrete mixture. The
slump value of concrete blended with 20% RHA (ground in a vibratory
mill for 120 min) was found to be 160 mm, which is 20 mm higher than
the control concrete. Concrete blended with 20% ground SCBA also
showed an improvement in the slump by 21.4% compared to the
reference concrete (Cordeiro et al., 2012). Regardless of the smaller
particle size of ground RHA, an improvement in the slump was observed
for the blended mixture compared to cement concrete by Givi et al. as
well. On grinding, the cellular structure of RHA was broken down, which
reduces the water demand and increases the workability with increasing
grinding time. Grinding beyond 120 min alters the cellular structure of
6
Journal of Cleaner Production 316 (2021) 128242
RHA (Aprianti et al., 2015). Another reason could be the adsorption of
RHA particles by oppositely charged cement particle surface, which
helps in preventing the flocculation of cement particles. This would have
otherwise trapped a considerable amount of mixing water, thereby
increasing the water demand (Givi et al., 2010). The study conducted by
Bakar et al. showed that the amount of water required to maintain a
similar slump was reduced as the grinding time was increased (Bakar
et al., 2011). This can be inferred from the decrease in SP dosage, as
depicted in Fig. 4. On the contrary, a higher slump was reported for a
concrete mixture containing 180 min ground RHA compared to 30 min
ground RHA owing to the greater SSA of ultra-fine particles after 180
min of grinding (Givi et al., 2010). However, Cordeiro et al. observed
that for concrete specimens with higher replacement levels of ground
RHA, the slump value was decreased because of greater demand for
water due to the high surface area and carbon content in RHA. Hence, to
achieve similar consistency as that of control concrete, a higher dosage
of superplasticisers will be required (Cordeiro et al., 2009a).
Fig. 4 shows an enhancement in slump and reduction of SP dosage
when as-received RHA was ground in a ball mill (Venkatanarayanan and
Rangaraju, 2015). Another study on ground RHA samples exhibited a
reduction in w/b ratio required for achieving the same value of slump as
the duration of grinding advanced (Rukzon et al., 2009). In the case of
ground POFA (GPOFA) blended concrete, there was an improvement in
the slump by 23% compared to the unground POFA (UPOFA) mixture
for 10% replacement (Jaturapitakkul et al., 2007). Besides, for 20%
replacement of cement with GPOFA, 5.3% increase in the slump
compared to OPC concrete was observed by Zeyad et al. Lower specific
gravity of GPOFA results in greater paste volume, better coating of ag­
gregates and filling of gaps between aggregates. This helps in improved
lubrication and inter aggregate mobility and thereby leads to enhanced
workability. However, for higher replacement levels, slump value was
found to be reduced owing to higher amounts of unburnt carbon, which
is responsible for steric repulsion as it absorbs a significant amount of SP
added to the mixture (Zeyad et al., 2016). The effect of grinding POFA
on the flowability of blended mortar was evident as the water
R. Rithuparna et al.
Fig. 4. Variation of fresh properties with change in the duration of grinding.
requirement to maintain ±5 the flow value of cement mortar was higher
as the particle size of GPOFA increased. The unground POFA blended
mortar with 40% replacement showed 24% higher water demand due to
irregular and porous particles (with D50 = 119.9 μm) of POFA. In
contrast, a similar flow as that of cement mortar was obtained for fine
POFA (D50 = 3 μm) blended mortar without adding extra water. This
can be attributed to the reduction in the porous structure of POFA after
grinding, which results in lesser water absorption and availability of
more water for blending the mix (Asrah et al., 2015).
Few researchers also studied the effect of grinding on initial and final
setting times of cement paste blended with ground RHA and SCBA
materials. Even though the paste with unground RHA (URHA) and paste
with ground RHA (GRHA) have comparable initial setting time, the final
setting time was increased by 40 min for URHA and 80 min for ground
RHA compared to control paste. This may be due to higher water ab­
sorption of porous URHA particles, which will reduce the effective w/b
ratio and increase the rate of hydration of cement and thereby affecting
the stiffening time of the paste (Venkatanarayanan and Rangaraju,
2015). However, Da Silva et al. observed that when the RHA sample was
ground, the paste had stiffened in lesser time compared to the paste with
URHA. This shows the greater reactivity of GRHA compared to URHA
(Da Silva et al., 2014). Paste with sieved and ground SCBA (GSCBA)
samples also showed a slight reduction in the setting time compared to
unground SCBA (USCBA) paste (Chopperla et al., 2019).
3.4. Influence of grinding time on strength of blended cementitious
systems
A significant improvement in the compressive strength of concrete
specimens with the ground AWAs compared to the unground ashes was
reported by the researchers, as clearly shown in Fig. 5 (a). The greater
strength for GRHA blended concrete is attributable to the higher reac­
tivity and better pore filling ability of the ground ash, which results in a
7
Journal of Cleaner Production 316 (2021) 128242
denser concrete (Bahri et al., 2018; Bakar et al., 2011; Xu et al., 2015).
This can be confirmed by the SEM analysis of the RHA particles, which
revealed that the microstructure of URHA is irregular and vesicular in
nature, whereas GRHA particles have a uniform and fine size, which
leads to an improved pozzolanic reaction (Venkatanarayanan and
Rangaraju, 2015). The reduction in the particle size of the ground RHA,
SCBA and POFA samples are clearly evident on comparing the micro­
structure of unground and ground AWAs shown in Fig. 5.
A direct relationship between Blaine’s fineness of SCBA particles and
strength was established, whereas the strength was inversely propor­
tional to the particle size of the ash particles (Cordeiro et al., 2008).
Ismail et al. observed an increased compressive strength of 58.6 MPa for
GPOFA blended concrete with a mean particle size of 10 μm compared to
54.8 MPa for 45 μm sample (Ismail et al., 2010). As the degree of
grinding was increased, the size of the particles was decreased, and there
was a corresponding improvement in the strength of GSCBA blended
specimens. Maximum compressive strength of 40.14 MPa was reported
for the specimen with ground material of SCBA particles passing through
53 μm and retained on 45 μm sieve (Bahurudeen and Santhanam, 2015).
A similar increase in the compressive strength of GSCBA blended con­
crete (108% higher than USCBA blended concrete) was observed when
the SCBA was ground in a vibratory mill for 240 min (Cordeiro et al.,
2009c).
An enhancement in the compressive strength by 30% was witnessed
for specimens with GPOFA compared to UPOFA in the study conducted
by Jaturapitakkul et al. The fineness of POFA particles is a crucial factor
which influences the compressive strength since POFA samples with
finer particles have greater pozzolanic reactivity as well as filler ability.
The optimum replacement level suggested for small sized POFA (D50 =
12.3 μm) is 30% which showed a compressive strength of 56 MPa. On
the other hand, mortar blended with medium (13 μm) and large sized
(30.8 μm) POFA particles reported the highest compressive strength of
51.7 MPa and 47.3 MPa, respectively for the 10% replacement of cement
R. Rithuparna et al. Journal of Cleaner Production 316 (2021) 128242

Fig. 5. Micrograph of ground and unground agro-waste ashes.

8
R. Rithuparna et al.
(Jaturapitakkul et al., 2011). Moreover, the higher porosity of UPOFA
increased the w/b ratio of the blended concrete and led to a decrease in
the strength (Jaturapitakkul et al., 2007). Nagaratnam et al. studied the
influence of ground POFA (ground to a size of approximately 13 μm
using a ball mill) as a cement replacement material along with fly ash.
Replacement of cement with 10% fly ash and 10% ground POFA
imparted a strength of 68 MPa and 60 MPa, respectively. Moreover, the
combined use in the ternary blended concrete with 5% POFA and 5% fly
ash led to a similar strength as that of binary blended concrete with 10%
POFA (Nagaratnam et al., 2019). It was reported that grinding WSA in a
combination of a ball mill for 45 min and a disintegrator mill at 30,000
rpm, 3 min for three cycles was more effective in improving the strength
of blended mortar than grinding WSA in a ball mill for 60 min (Qudoos
et al., 2020). Hence, it can be stated that the duration of grinding
adopted will significantly influence the properties of the materials.
Fig. 6 (b) represents the variation of normalised compressive
strength of specimen blended with ground AWAs with respect to un­
ground ashes for different grinding time. It can be noticed that all the
ground samples based concrete exhibited better performance than the
reference concrete, although there is an optimal time for which the
strength gain was maximum. The optimum duration for grinding is
governed by the source from which RHA was received and the grinding
conditions adopted for obtaining the ground ash. For the RHA obtained
by burning rice husk in a gas furnace at 700 ◦ C for 6 h, 90 min was found
to be the optimum duration of grinding in a ball mill at 76 rpm (Bakar
et al., 2011). Whereas for RHA received from an electronic furnace after
calcination of rice husk at 600 ◦ C for 2 h, 30 min of grinding in a ball mill
at 1000 rpm was reported for better compressive strength (Xu et al.,
2015). The reason stated is the lowest water requirement and highest
pozzolanic reactivity that were achieved after grinding the RHA for the
corresponding optimum duration (Bakar et al., 2011). For concrete
specimens blended with GSCBA samples, as the grinding time of SCBA
increased from 30 to 240 min, a significant increase in the compressive
strength by 30% was observed. The progressive increase in the packing
density with an increase in the duration of grinding was stated as the
reason for the enhancement in strength. This can be attributed to the
filling of interstices between coarse particles by the ultrafine SCBA
particles (Cordeiro et al., 2008). The addition of ground RHA (20 μm)
and ground SCBA (17 μm) along with fly ash as a cement replacement
material was studied by Rukzon and Chindaprasirt. A marginal
enhancement in the compressive strength compared to the SCBA based
binary concrete was reported. A similar observation was also witnessed
Fig. 6. Compressive strength of blended concrete specimens: (a) Comparison of unground and ground samples; (b) Variation with respect to grinding time.
9
Journal of Cleaner Production 316 (2021) 128242
for RHA blended binary concrete. Therefore, ternary blends with
agro-industrial wastes are found to be more effective than binary blends
(Rukzon and Chindaprasirt, 2014).
From Table 1, it can be inferred that grinding of ash particles does
not have much influence on the splitting tensile and flexural strength of
blended concrete specimens. Compared to control concrete, the increase
in tensile strength after 28 days of curing was only 5% when the RHA
ground in a ball mill was incorporated in the concrete (Venkatanar­
ayanan and Rangaraju, 2015). For GPOFA concrete as well, there was
only a slight improvement in the tensile strength as a result of grinding
(Ismail et al., 2010). Although the tensile strength of concrete incorpo­
rating U-BRHA with porous structure was lower than control concrete,
the strength was improved to 118% of control concrete after grinding.
Similarly, for control burnt RHA, there was an increase in tensile
strength from 1.22 to 1.36 times that of control concrete. Better bond
strength of concrete owing to the higher rate of pozzolanic reaction and
more amount of CSH formation may be the reason for this improvement
in strength. Compared to GRHA, however, G-BRHA had lower strength
due to its higher carbon content and lower amount of reactive silica
content (Bahri et al., 2018). The effect of grinding of RHA on flexural
strength was minimal, only 1% and 7% increase in strength for 7.5% and
15% replacement of cement with GRHA, respectively, were reported
(Venkatanarayanan and Rangaraju, 2015). Similar results were also
reported by Jamil et al. on 10% and 20% replacement of cement with
GRHA (Jamil et al., 2016). Approximately equal strength in flexure as
that of control concrete was observed on replacing cement partially with
WSA, which was ground for 60 min in a ball mill (Qudoos et al., 2020).
3.5. Influence of grinding time on durability properties of blended
cementitious systems
Studies on the influence of grinding on durability properties of AWAs
blended concrete are limited. Fig. 7 represents the relative difference in
water absorption of blended concrete with respect to control concrete.
Relative difference is calculated as the ratio of difference in water ab­
sorption (water absorption of control – water absorption of blended
concrete) to the water absorption of control specimens. The water ab­
sorption of concrete with 60 min ground RHA was higher than that of
control concrete for 10% replacement of cement. The hygroscopic na­
ture of coarse RHA particles is the reason for the increase in water ab­
sorption. Moreover, for 20% replacement of the cement with 60 min
ground sample, the relative difference is even higher due to the dilution
R. Rithuparna et al. Journal of Cleaner Production 316 (2021) 128242

Table 1
Influence of grinding on splitting tensile and flexural strength of blended specimens.
Material Grinding condition Specimen Tensile strength Flexural strength Reference
(MPa) (MPa)

RHA Ash received from furnace was ground in a planetary ball mill Cement 2.72 5.17 Venkatanarayanan and Rangaraju
operated at a speed of 250 rpm concrete (2015)
7.5% U-RHA 3.14 5.53
7.5% G-RHA 3.29 5.61
15% U-RHA 2.82 5.87
15% G-RHA 3.13 6.20
RHA Ash was ground in Los Angeles abrasion machine at 30–33 rpm Cement mortar – 8.80 Jamil et al. (2016)
10% G-RHA – 9.60
20% G-RHA – 10.00
RHA BRHA and controlled burnt RHA were ground in Los Angeles 20% U-BRHA 3.20 – Bahri et al. (2018)
machine for 16 h and 30,000 cycles 20% G-BRHA 4.40 –
20% U-RHA 4.60 –
20% G-RHA 5.10 –
POFA POFA was sieved through 300 μm sieve before grinding Cement 4.36 – Ismail et al. (2010)
Concrete
20% 45 μm 4.40 –
POFA
20% 10 μm 4.74 –
POFA
WSA As-received ash was ground in ball mill at 350 rpm for 60 min Cement mortar – 9.10 Qudoos et al. (2020)
20% G-WSA – 9.25

Fig. 7. Relative difference in water absorption for blended concrete (grinding time is mentioned in the graph).

effect. On the other hand, the degree of absorption was found to reduce
for the concrete with 10% replacement of cement with 90 min ground
RHA as a result of improved reactivity and lower availability of
permeable pores owing to higher fineness and filler effect of the fine
RHA particles. There was a further reduction when the replacement
level was 20% due to increased production of secondary CSH (Givi et al.,
2010; Jamil et al., 2016). In a similar way, for concrete with 15% RHA
ground for 30 min, there was 8% increase in water absorption, whereas
for ultrafine RHA (180 min) blended concrete, a reduction in the water
absorption by 5.7% was noticed. Another observation made was the
improvement in the interfacial transition zone due to the higher amount
of hydration products and better pore filling ability of ultrafine RHA
(Givi et al., 2010). Comparing concrete blended with URHA and GRHA,
a significant reduction in the absorption of water can be detected on the
addition of ground RHA, and there was a further improvement on the
higher dosage level of RHA. The faster hydration of finer particles of
GRHA results in a less permeable matrix which is accountable for lower
water absorption (Venkatanarayanan and Rangaraju, 2015).
Resistance to chloride penetration is another important durability
parameter which affects the performance of concrete. The rapid chloride
permeability test (RCPT) is a widely used method to measure the total
electric charges passed through the concrete specimen under a constant
applied voltage. The total charges passed depends on the permeability of
concrete and the composition of the pore solution present in it (Ven­
katanarayanan and Rangaraju, 2015). The results of the RCPT con­
ducted in various studies are shown in Fig. 8. It can be observed that all

10
R. Rithuparna et al.
Fig. 8. Total charges passed for unground and ground concrete specimens.
the concrete incorporating ground ashes can be classified under the
category of very low permeability concrete since the total charges
passed through the specimens were well below the mark of 1000 Cou­
lombs. A remarkable reduction in the total charges passed was observed
for GRHA blended concrete than control concrete till 15% of cement
replacement. This reduction was attributed to the pozzolanic reactivity
of GRHA and subsequent pore refinement in GRHA blended concrete.
Besides, the finer size of GRHA resulted in the filler effect and reduced
the permeability of concrete. On the other hand, earlier literature stated
10–20% of RHA as the optimum replacement level in concrete. Hence,
beyond 15%, the dilution effect was occurred and led to a reduction in
the compressive strength and durability (Chindaprasirt and Rukzon,
2008; Da Silva et al., 2008; Ganesan et al., 2008; Saraswathy and Song,
2007). Therefore, there is no significant reduction in the permeability
and only less variation was observed between 15% and 20% replace­
ment level of cement with GRHA. Bahri et al. studied the effect of
grinding on chloride permeability of high carbon (BRHA) and low car­
bon RHA (RHA) incorporated concrete. After 28 days of curing, the total
charges passed for U-BRHA was 108% of control concrete; however, it
can still be classified as a good quality concrete as per ASTM C1202
(2012). The high LOI content and coarser BRHA particles (165 μm) may
be the reasons for the higher electrical conductivity. The value was
increased by 1.25 times when the BRHA particles were ground to a
fineness of 67 μm. Moreover, a reduction in the total charges passed
were found for low carbon RHA blended concrete specimens (Bahri
et al., 2018). In another study, the specimen blended with 7.5% URHA
falls into the category of concrete with low permeability, whereas the
specimen with 7.5% GRHA falls into very low permeability category.
This reduction in the permeability can be attributed to the denser matrix
of GRHA blended concrete as a result of the higher reactivity of fine
GRHA particles. Besides, a discontinuity in the internal porosity created
by coarse RHA particles was observed for GRHA mixed concrete causes a
reduction in the permeability of concrete (Venkatanarayanan and Ran­
garaju, 2015).
The total charges passed through concrete blended with 20% GSCBA
was 5832 Coulombs (high chloride ion permeability), whereas it was
2862 Coulombs (moderate chloride ion permeability) for ternary
blended concrete with 20% GRHA and 20% GSCBA. Moreover, the 20%
GRHA blended concrete falls under the category of low chloride ion
permeability with 88% reduction in the total charges passed compared
to the control concrete. A notable increase in the chloride resistance of
GRHA blended concrete can be attributed to the higher pozzolanic
reactivity of GRHA than GSCBA (ASTM C1202, 2012; Cordeiro et al.,
2012). A significant reduction in the total charges passes through 15%
11
Journal of Cleaner Production 316 (2021) 128242
GSCBA blended concrete (774 Coulombs indicating very low chloride
penetration) compared to the control concrete (1179 Coulombs) was
observed when SCBA was ground for 240 min (Cordeiro et al., 2009c).
Ismail et al. studied the depth of chloride penetration for GPOFA (with a
mean particle size of 10 μm) blended concrete. The observed depths of
chloride penetration were 12 mm and 5.5 mm for control and GPOFA
blended concrete, respectively (Ismail et al., 2010).
Some of the other properties investigated by various researchers
include resistance to acid attack and sulfate attack. Deterioration of
concrete by sulfates present in soil, groundwater or seawater is a pri­
mary concern as it reacts with C3A and Ca(OH)2 present in the concrete,
leading to expansion, cracking and reduction of strength. A study on
concrete specimens when exposed to 5% MgSO4 revealed that there was
a reduction in the expansion by 13.6% for 30% GPOFA blended concrete
compared to the concrete with 30% UPOFA. The improved pozzolanic
reaction of GPOFA resulted in better pore refinement, highly imper­
meable matrix and reduction in the amount of CH availability. In
addition, the higher the fineness of POFA, the lower was the expansion
of concrete since finer POFA acts as a filler and makes the concrete less
porous and denser (Jaturapitakkul et al., 2007). The influence of fine­
ness of GPOFA on the resistance of concrete to acid attack was studied by
Ismail et al. The study revealed that since the acid mainly attacks hy­
drated lime in the matrix, GPOFA reacts with most of the CH present and
its addition in concrete results in better resistance to acid attack.
Moreover, GPOFA with 10 μm size reacts more compared to GPOFA with
45 μm size, thus producing a further amount of CSH, which will fill the
pores in the matrix (Ismail et al., 2010).
4. Thermal processing
4.1. Influence of burning on LOI and colour of the ashes
Loss on ignition (LOI) is primarily a measure of the amount of un­
burnt carbon content and volatile matter present in the ash, and its
colour gives an indirect indication of the quality of the burnt ash. The
dark colour is mainly due to the presence of unburnt carbon in the ash,
which will affect both the pozzolanic reactivity as well as the work­
ability of the concrete (Memon et al., 2018). The maximum limit of LOI
specified in ASTM C618 for natural pozzolans is 10% (ASTM C618,
2019). From Fig. 9, it can be depicted that the burning temperature has a
significant influence on the LOI value of the AWAs. The general trend
noticed on increasing the temperature is a reduction in the carbon
content, which leads to low LOI. A change in the colour of the burnt RHA
from white-grey to pinkish-white was observed when the degree of
burning was increased from 600 ◦ C to 1000 ◦ C (Jaya et al., 2013). This
transition in colour is because of the reduction in the unburnt carbon
content of the ash. Similarly, when the duration of burning at 600 ◦ C was
increased from 1 h to 2 h, the RHA changed from light grey to slightly
white in colour, and there was a reduction in the LOI value, as shown in
Table 2. However, when the temperature was increased to 700 ◦ C, some
black particles were noticed in the ash, which is due to the presence of
unburnt carbon. Hence, the loss on ignition was higher for RHA burnt at
700 ◦ C (Bie et al., 2015). Once the burning temperature reaches the
decomposition temperature of potassium oxide (K2O) present in the
pozzolan, it will melt and trap the residual carbon particles. This results
in incomplete burning of the carbon particles and thereby gives a black
appearance to the RHA (Krishnarao et al., 2001). The influence of the
burning duration of RHA was investigated by Nair et al., as shown in
Table 2. It can be noted that at 900 ◦ C, burning for 6 h sufficiently
remove the unburnt carbon, whereas for burning at 500 ◦ C and 700 ◦ C,
12 h were required to lower the LOI below the permissible value as per
the ASTM standard (ASTM C618, 2019). However, more than 50% of the
organic content remained in the ash when it was burnt at 300 ◦ C for 24
h. Therefore, burning at lower temperatures and for shorter durations
were not effective in reducing the LOI of the RHA samples (Nair et al.,
2008).
R. Rithuparna et al. Journal of Cleaner Production 316 (2021) 128242

Fig. 9. Variation of loss on ignition with burning temperature.

The RHA samples obtained from different burning temperatures of

Table 2
600 ◦ C, 800 ◦ C and 1000 ◦ C had LOI values ranging from 0.9 to 2.4%,
Variation of LOI with respect to burning temperature and duration.
which were found to be within the acceptable limit (Jaya et al., 2013).
Material Burning Burning Burning LOI Reference Similarly, Lo et al. studied the influence of burning temperature on the
condition temp. duration (%)
removal of unburnt carbon in RHA. The LOI values of RHA burnt at
(◦ C) (min)
550 ◦ C, 700 ◦ C and 900 ◦ C for 4 h in a furnace were found to be 5.38,
RHA Ashes were 300 ◦ C 1440 53 Nair et al. (2008) 2.42 and 0.5%, respectively (Lo et al., 2020). The RHA burnt in a
prepared by 500 ◦ C 360 32
burning rice 720 4
specially designed furnace had a high LOI at lower temperatures
husk in a 1440 5 whereas, at a temperature beyond 650 ◦ C, the LOI of the sample was
laboratory 700 ◦ C 360 6 considerably reduced to less than 6% (Ramezanianpour et al., 2009).
oven with 720 2 Likewise, a reduction in the LOI was observed for SCBA samples on
continuous air 1440 1
increasing the burning temperature. Murugesan et al. stated the effect of
supply 900 ◦ C 360 1
720 0.5 processing on LOI of SCBA and found it to vary from 3% to 8% in most of
RHA Combustion 550 ◦ C 60 21.01 Ramezanianpour the earlier research studies. However, unprocessed SCBA has an LOI
of rice husk 90 14.95 et al. (2009) greater than the permissible limit of natural pozzolan (Murugesan et al.,
was carried 600 ◦ C 60 15.33 2021). Cordeiro et al. reported that burning up to 600 ◦ C was adequate
out in a 90 9.81
specially 650 ◦ C 30 19.53
to remove reasonable amounts of residual carbon such that the LOI was
designed 60 5.91 only 5.7% (Cordeiro et al., 2009b). The presence of fibrous carbon
furnace 90 5.48 particles in SCBA was stated as the reason for higher LOI at lower
700 ◦ C 30 14.53 temperatures of burning. In addition, the colour of ash changed from
60 6.01
extreme black to grey as the degree of burning was increased. This can
90 4.14
750 ◦ C 30 12.09 be attributed to the crystallisation and thermal decomposition of the ash
60 2.67 at higher temperatures (Bahurudeen and Santhanam, 2015). Better
RHA Rice husk was 25 9.02 Vayghan et al. calcination of WSA at higher temperatures was the reason for the
heated in a 700 ◦ C 60 1.72 (2013) reduction in the observed LOI when the burning temperature of WSA
muffle 240 1.28
furnace at a
was increased. The LOI was found to be decreased from 12.8% to 5.8%
rate of 10 ◦ C/ for the WSA burnt from 500 ◦ C to 600 ◦ C, which shows that a significant
min amount of carbon was oxidised (Memon et al., 2018). A similar reduc­
RHA Rice husk was 600 ◦ C 60 1.52 Bie et al. (2015) tion in LOI from 8.55% to 3.98% was noticed in the case of BLA on
thermally 120 1.48
increasing the calcination temperature from 500 ◦ C to 700 ◦ C. Moreover,
treated in a
muffle the increase in silica content from 71.77% to 74.7% was also stated for
furnace at a calcined BLA (Villar-Cociña et al., 2018). The reduction in unburnt
rate of 5 ◦ C/ carbon content can be attributed to the volatilisation of potassium-based
min compounds on calcining BLA at higher temperatures (Roselló et al.,
2015). In another study, SCBA and BLA were initially burnt at 400 ◦ C for
60 min and later calcined at 700 ◦ C and 600 ◦ C for 60 min, respectively.

12
R. Rithuparna et al.
The LOI values of SCBA (5.37%) and BLA (7.79%) were reported to be
lower than the specified limit for natural pozzolans (Rodier et al., 2019).
4.2. Influence of burning on pozzolanic reactivity
Pozzolanic reactivity is predominantly governed by the amount of
amorphous silica and carbon content in the ash. It is clearly shown in
Fig. 10 that the PAI was lower when burnt at lower temperatures,
reached a maximum value at an optimum temperature and decreased
thereafter on further increasing the temperature. A similar trend was
observed for Chapelle activity as well, irrespective of the material
considered for the study. The presence of unburnt carbon at lower
burning temperatures and the formation of crystalline silica at higher
temperatures are accountable for this variation in the pozzolanic reac­
tivity of the AWAs (Cordeiro et al., 2009b; Memon et al., 2018, 2020,
2020; Memon and Khan, 2018). The presence of unburnt carbon will
affect the hydration of cement and increase the water demand due to
their porous structure, thereby decreasing the strength of the cementi­
tious system. The carbon and volatile matter were significantly removed
at a temperature of 600 ◦ C for SCBA (Cordeiro et al., 2009b), whereas for
CCA and corn stalk ash (CSA), the optimum burning temperature was
500 ◦ C, at which maximum PAI values of 97.3% and 98.6%, respec­
tively, were achieved (Memon et al., 2020; Memon and Khan, 2018). As
shown in Fig. 10, the PAI value was well above the minimum require­
ment as per the ASTM standard on burning the ash samples at the cor­
responding optimum temperatures (ASTM C618, 2019).
For SCBA, burning in an electric oven for 90 min, the reactivity was
found to be reduced beyond 700 ◦ C owing to the recrystallisation of
cristobalite (Bahurudeen and Santhanam, 2015). In a similar way, the
optimum temperature for WSA was 600 ◦ C, below which the reactivity
was found to be less as a result of high LOI. For WSA burnt at 600 ◦ C, the
maximum PAI value determined was 85.2%, and the Chapelle activity
was 453.5 mg/g, which is relatively higher than the standard value of
330 mg/g as specified in the French Norm NF P 18–513 (NF P 18 513,
Fig. 10. Comparison of PAI and Chapelle activity for different burning temperatures.
13
Journal of Cleaner Production 316 (2021) 128242
2012). Beyond that temperature, the amorphous silica gets converted
into crystalline phases, which makes the material less reactive in nature
(Memon et al., 2018). Similarly, the Chapelle activity index of the BLA
burnt at 600 ◦ C for 3 h was stated to be 345 mg/g, which is more than the
minimum requirement (Rodier et al., 2017).
In addition to pozzolanic activity index and Chapelle activity, kinetic
coefficients can also be used to evaluate the pozzolanic reactivity of
supplementary cementitious materials. Kinetic coefficients, primarily,
the reaction rate constant was determined using kinetic–diffusive model
proposed by Villar-Cocina et al. (Villar-Cociña et al., 2003). Decreasing
nucleus model was used by Villar-Cocina et al. to form the kinet­
ic–diffusive model (Villar-Cociña et al., 2003). To evaluate the reaction
rate from the model, the conductivity of AWA-lime solution was
measured. As shown in Fig. 11 (a), SCSA calcined at 800 ◦ C has a higher
reaction rate than calcined RHA (800 ◦ C) and SCSA (1000 ◦ C). The re­
action rate is a direct indication of pozzolanic reactivity. The increase in
the calcination temperature decreased the reaction rate by reason of the
formation of crystalline silica at higher temperature (Frías et al., 2007).
Moreover, the reaction rate of the SCSA-CH system is higher than
SCBA-CH system, signifying higher reactivity for SCSA calcined at
800 ◦ C compared to SCBA calcined at the same temperature
(Villar-Cociña et al., 2008). A similar result was reported by Morales
et al. It was also stated that for both SCBA and SCSA, reaction rate de­
creases with an increase in the calcination temperature (Morales et al.,
2009). It was reported that SCBA calcined at 800 ◦ C exhibited a higher
reaction rate even at early ages, unlike SCBA calcined at 1000 ◦ C as
shown in Fig. 11 (a) (Villar-Cociña et al., 2009). Rodier et al. compared
the reaction rate of SCBA burnt at 700 ◦ C and BLA burnt at 600 ◦ C. The
reaction rate of BLA (100.2 × 10− 2) was found to be remarkably higher
than the reaction rate of SCBA (1.85 × 10− 2) (Rodier et al., 2019). The
BLA burnt at 600 ◦ C was noted to have a higher reaction rate (8.41 ×
10− 1 h− 1) owing to its higher pozzolanic reactivity in comparison with
SCBA, and SCSA burnt at 800 ◦ C (Villar-Cociña et al., 2011). Moreover,
the reaction kinetics of the BLA-CH system was examined for two
R. Rithuparna et al.
Fig. 11. Effect of burning temperature on reaction kinetics of AWAs.
differently calcined BLA (calcined at 600 ◦ C and 700 ◦ C), and their re­
action rates were obtained to be comparable. However, on increasing
the calcination temperature further, the reaction rate of the system was
declined significantly (Villar-Cociña et al., 2018). Similar to that of PAI
and Chapelle activity, the reaction rate was also found to decrease with
the increase in the calcination temperature.
One of the most important parameters that characterise the pozzo­
lanic reactivity of the supplementary cementitious materials is the
thermodynamic parameter of activation called free energy of activation.
The free energy of activation is calculated using the Eyring equation.
Higher free energy of activation leads to stable kinetics and indicates
low reactivity of SCM. As shown in Fig. 11 (b), the SCBA-lime system
(SCBA calcined at 800 ◦ C) has higher activation energy than SCSA-lime
(SCSA calcined at 800 ◦ C), specifying the lower reactivity of SCBA
(Villar-Cociña et al., 2008). As free energy of activation is directly
related to the pozzolanic reactivity, increasing calcination temperature
of SCBA decrease the reactivity of SCBA (Fig. 11 (b)) (Villar-Cociña
et al., 2009). As evident in Fig. 11 (b), kinetic instability was reported for
BLA burnt at 600 ◦ C, referring to its higher reactivity (Villar-Cociña
et al., 2011). In addition, the stability of the system was stated to in­
crease with an increase in the calcination temperature of BLA to 800 ◦ C
(Villar-Cociña et al., 2018). It can be inferred that stable kinetics was
evident when agro-waste ashes are calcined at a higher temperature.
4.3. Influence of burning on mineralogical characteristics
The XRD analysis is carried out to identify the crystalline phases for
different burning temperatures and durations. In general, the major
crystalline compounds present in the agro-wastes ashes, such as RHA,
SCBA, POFA etc., were quartz, cristobalite, kaolinite, and gibbsite based
on the X-ray diffraction study (He et al., 2020). The diffraction pattern of
RSA burnt at 450 ◦ C, 550 ◦ C, and 650 ◦ C showed an amorphous hump in
the range of 15–30◦ (2θ). An interesting point to note is the total absence
of peaks corresponding to crystalline silica forms such as cristobalite and
trydimite, which signifies that crystallisation of silica does not take place
within the above mentioned temperature range (Roselló et al., 2017).
Similarly, broad peaks in the XRD pattern of RHA burnt at 500 ◦ C, and
700 ◦ C indicates the amorphous nature of silica present in RHA. In
contrast, after 900 ◦ C of burning, sharp and intense peaks were observed
owing to the formation of crystalline cristobalite. The XRD pattern of
RHA burnt at 1100 ◦ C exhibited a further increase in the number of
sharp peaks because of the formation of cristobalite and tridymite
crystals (Nair et al., 2008). In another study of RHA calcined at different
temperatures, the diffraction pattern of RHA burnt at 600 ◦ C showed
broad peaks indicating amorphous silica, whereas at calcination tem­
peratures above 700 ◦ C, sharp peaks corresponding to crystalline phases
14
Journal of Cleaner Production 316 (2021) 128242
of silica such as quartz (2θ = 26.7◦ ) for 700 ◦ C burnt RHA, cristobalite
(2θ = 22.5◦ ) and tridymite (2θ = 26◦ ) for 900 ◦ C burnt RHA were
detected (Xu et al., 2018). Moreover, prolonged periods of burning the
RHA above 650 ◦ C was reported to reduce the amorphous silica content.
Hence, at higher temperatures as well as for longer durations of burning,
the reactivity of RHA is reduced as a result of the transformation of the
amorphous silica to crystalline form (Ramezanianpour et al., 2009). In a
similar way, the crystalline silica was detected in the diffraction pattern
on calcining WSA and SCBA over a temperature greater than 700 ◦ C
(Bahurudeen and Santhanam, 2015; Memon et al., 2018). At 800 ◦ C,
cristobalites were detected in the SCBA sample, and at 1100 ◦ C, in
addition to cristobalites, tridymites were formed. As the degree of
burning was increased, a higher amount of prismatic and spherical
particles were identified, and there was a lesser number of fibrous car­
bon particles in the micrograph of the burnt SCBA sample (Bahurudeen
and Santhanam, 2015).
The XRD patterns of SCSA burnt at 800 ◦ C, and 1000 ◦ C showed small
humps in a broad region between 15◦ and 35◦ indicating the presence of
amorphous phases. The main crystalline compound identified for SCSA
burnt at 800 ◦ C was calcite, whereas it was alpha cristobalite for SCSA
burnt at 1000 ◦ C. Thereby implying that the amorphous silica content
was more in SCSA burnt at 800 ◦ C than SCSA burnt at 1000 ◦ C (Morales
et al., 2009). In the diffractogram of maize stalk leaf ash, the peaks of
cristobalite was detected only when the burning temperature was above
850 ◦ C, whereas quartz peaks were present in the diffractogram of ashes
burnt at 500 ◦ C, 700 ◦ C and 850 ◦ C. The early formation of cristobalite
may be due to the presence of alkali metals in the maize stalk leaf ash,
which will accelerate the crystallisation of silica (Feng et al., 2019). An
amorphous hump was detected in the XRD diffractogram of calcined
BLA (burnt at 600 ◦ C for 2 h) by Dwivedi et al. Similar observation is also
reported by Singh et al. (Dwivedi et al., 2006; Singh et al., 2007). In the
temperature range of 500 to 700 ◦ C, the effect of calcination tempera­
ture on the mineralogical characteristics of BLA was not much signifi­
cant. However, for BLA calcined beyond 700 ◦ C, cristobalite was
detected at a 2θ value of 21.9◦ (Villar-Cociña et al., 2018). A study of the
X-ray pattern of CCA at different incineration temperatures has revealed
broad peaks at 2θ values in the range of 30–35◦ up to 600 ◦ C. After­
wards, several sharp peaks at 30.68◦ (stishovite) and 32.37◦ (cristoba­
lite) were observed, evidencing the crystalline nature of silica (Memon
and Khan, 2018). Likewise, for CSA, the intense peaks of quartz started
to appear at 2θ of 26.51◦ on burning at 600 ◦ C, and cristobalite peaks at
2θ of 29.38◦ for 700 ◦ C burnt ash (Memon et al., 2020). Hence, the
burning process will be effective in improving the pozzolanic reactivity
only up to an optimum temperature, after which the amorphous silica
gets transformed into a crystalline phase for all the AWAs that were
reported.
R. Rithuparna et al.
4.4. Influence of burning on fresh properties of blended cementitious
systems
Some of the factors which influence the workability of the blended
cementitious system are the carbon content in the material and fineness.
From sections 4.1 and 4.3, it can be inferred that the burning temper­
ature has a significant influence on the LOI and the phase of silica in the
material. Hence, the temperature at which the ashes are burnt will
indirectly affect the flow characteristics of the AWA blended mixtures.
The presence of high unburnt carbon content in untreated SCBA (>10%)
was reported to adversely affect the workability of SCBA blended con­
crete and pozzolanicity of SCBA. However, calcination under controlled
condition was helpful to obtain more reactive SCBA with a desirable
range of LOI, thereby improving the workability of processed SCBA
blended concrete (Murugesan et al., 2021). The influence of thermal
treatment on the flow characteristics of RSA, which was produced by
uncontrolled burning, was studied by Munshi and Sharma. The results
revealed that the RSA burnt in uncontrolled conditions had poor slump
flow owing to high carbon content and improper burning of organic
matter present in the residual ash. There was a slight improvement in the
workability, as the open burnt RSA was treated in a muffle furnace at
400 ◦ C. Moreover, on burning the ash above 600 ◦ C, flow equivalent to
or greater than the control mortar was noticed (Munshi and Sharma,
2018). Similarly, the slump was increased from 145 mm to 170 mm
when the cement was replaced with 12.5% of RHA burnt at 750 ◦ C and
830 ◦ C, respectively (Nehdi et al., 2003). However, higher water de­
mand was observed in the case of RHA-fly ash blended ternary system
owing to the high fineness of calcined RHA at 600 ◦ C, which led to an
increase in the specific surface area of RHA (Medina et al., 2018). On
studying the consistency of CSA blended pastes, it can be observed that
the values were higher for all the CSA blended pastes compared to
Fig. 12. Normalised compressive strength of blended specimens for different burning temperature.
15
Journal of Cleaner Production 316 (2021) 128242
control paste. However, a decreasing trend was observed as the calci­
nation temperature was increased beyond 500 ◦ C. The reason for the
decrease is the crystallisation of CSA at a higher temperature which
smoothens the internal surfaces of the ash and results in a decrease in
water absorption capacity (Memon et al., 2020). Likewise, the consis­
tency of CCA blended paste was found to be decreased from 33 to 26% as
the degree of burning was increased from 400 ◦ C to 800 ◦ C and also the
value was below that of control paste for 800 ◦ C burnt CSA blended paste
(Memon and Khan, 2018).
4.5. Influence of burning on strength of blended cementitious systems
The researchers have reported a direct correlation between the
pozzolanic reactivity of material and the compressive strength of the
blended cementitious system. Hence, the factors which affect the poz­
zolanicity of a material, such as carbon content and amorphous silica
content, will influence the strength characteristics. For CCA and CSA, an
optimum burning temperature of 500 ◦ C was reported for which
maximum compressive strength of 35.75 MPa and 37.75 MPa, respec­
tively, was achieved for the blended concrete. The ashes burnt at 500 ◦ C
had lesser amounts of unburnt carbon and were rich in amorphous silica
compared to the ashes burnt at 400 ◦ C. After which, a subsequent
reduction in the strength was observed owing to the crystallisation of
silica, as confirmed in the X-ray diffraction analysis (Memon et al., 2020;
Memon and Khan, 2018). Fig. 12 shows that the compressive strength of
mortar incorporating RSA incinerated at different temperatures of
400 ◦ C, 600 ◦ C and 750 ◦ C, and the observed values were higher
compared to that of control mortar, owing to the high reactivity and
filler effect of the fine RSA particles (Munshi and Sharma, 2018).
For RHA blended concrete, there was no significant difference in the
compressive strength when the cement was replaced with 10% of RHA
R. Rithuparna et al.
burnt in a Torbed reactor at 750 ◦ C and 830 ◦ C, whereas for 12.5%
replacement, a slight reduction in the strength was noted. However, the
normalised compressive strength with respect to control concrete was
greater than one in all the cases, as presented in Fig. 12 (Nehdi et al.,
2003). However, compared to concrete mixed with RHA burnt at 600 ◦ C,
the compressive strength was found to be notably reduced for blended
concrete with RHA burnt at 700 ◦ C. This reduction in strength by 21%
was due to the presence of inactive crystalline silica. At higher
replacement levels, there was a further drop in the compressive strength
which can be attributed to the dilution effect (Bie et al., 2015). A
comparison of RHA produced by open burning and controlled burning
was presented in a study by Muthukrishnan et al., and the compressive
strength was reported to increase from 58 MPa to 63 MPa. Moreover, the
strength was improved by 24% when the uncontrolled RHA was ther­
mally treated at 425 ◦ C. This can be attributed to the complete oxidation
of unburnt carbon and the removal of K2O coating, which results in the
exposure of silica in the material (Muthukrishnan et al., 2019).
Furthermore, the combined use of processed RHA and fly ash was
examined by Medina et al. The RHA was calcined at four stages: i)
initially burnt at 10 ◦ C/min for 40 min, ii) 400 ◦ C for additional 25 min,
iii)10 ◦ C/min for 25 min and iv) 600 ◦ C for 2 h. The combined utilisation
of RHA and fly ash enhanced the strength of blended concrete. The early
age strength attainment of fly ash blended concrete is lesser than control
concrete. Incorporation of processed RHA with fly ash improved early
age strength (Jittin et al., 2021; Medina et al., 2018). In another study,
the addition of 10% and 20% BLA calcined at 600 ◦ C as a replacement
material for cement was investigated. The compressive strength of
blended mortar was found to increase from 36 MPa (control) to 40 MPa
(10%) and 44 MPa (20%), correspondingly (Rodier et al., 2019).
Moreover, combined utilisation of processed SCBA and BLA was studied
by Rodier et al. Initially, SCBA and BLA were calcined at 400 ◦ C for 60
min. Afterwards, further calcination was adopted at 600 ◦ C (SCBA) and
700 ◦ C (BLA) for 60 min. The compressive strength of the ternary
blended mortar with 10% SCBA and 10% BLA was higher than the bi­
nary blended mortar with 10% BLA (Rodier et al., 2019).
Few earlier studies are available on the effect of burning temperature
on flexural and tensile strength of concrete incorporating AWA. For
concrete with RHA obtained at 600 ◦ C of burning, the flexural strength
was reported to be maximum for 10% replacement. The flexural strength
was marginally higher for concrete with RHA burnt at 600 ◦ C for 2 h
compared to 1 h. Similar flexural strength was witnessed for 700 ◦ C
burnt RHA based concrete (Bie et al., 2015). On comparing the flexural
strength of open burnt RHA blended concrete with control, there was a
noticeable reduction in the strength due to its porous structure, which
weakens the tensile plane of mortar and facilitates the propagation of
cracks. However, there was a minor increase in the flexural strength
when the open burnt RHA was thermally treated at 425 ◦ C (Muthuk­
rishnan et al., 2019). The tensile strength of RHA blended concrete (RHA
was burnt at 650 ◦ C for 60 min) was reported to be 13% higher than that
of control concrete (Ramezanianpour et al., 2009).
5. Thermomechanical treatment
5.1. Influence of thermomechanical treatment on particle size and specific
surface area
In this section, the combined effect of mechanical and thermal
treatment on particle size and SSA is discussed and compared with
materials that have undergone only a single processing method. A slight
increase in the particle size was observed when the ground CCA was
further heated from 200 ◦ C to 600 ◦ C for 4 h. The micrographs of burnt
CCA samples at different temperatures revealed that the smaller parti­
cles melted to form larger particles. Besides, the agglomeration effect
was enhanced as the temperature of burning was increased. A corre­
sponding decrease in the surface area of the particles from 9050 m2/kg
to 7441 m2/kg was noted (Suwanmaneechot et al., 2015). However, an
16
Journal of Cleaner Production 316 (2021) 128242
increase in Blaine’s fineness was reported when CCA and CSA burnt at
500 ◦ C was further ground in a ball mill for 60 min and 120 min,
respectively, as shown in Fig. 13 (Memon et al., 2020; Memon and Khan,
2018). The combined effect of controlled recalcination (600 ◦ C for 60
min) and grinding of SCBA on the particle size was found to reduce the
particle size of SCBA significantly. The D50 value was reported to
decrease from 30 μm (raw SCBA) to 10 μm when the SCBA was ther­
momechanically processed (Cordeiro et al., 2019).
Heat treatment of sieved and ground POFA at 500 ◦ C for 90 min and
further grinding it in a ball mill to obtain ultrafine POFA resulted in an
increase in SSA by 35% (Zeyad et al., 2016). A similar increase in the
nitrogen adsorption from 4900 m2/kg to 7400 m2/kg was observed
when GPOFA was burnt at 600 ◦ C for 2 h in an electric furnace and then
further ground to a smaller size. (Alsubari et al., 2015). In the same way,
Blaine’s fineness for WSA calcined at 600 ◦ C was increased from 248 to
367 m2/kg by grinding for 120 min (Memon et al., 2018). After the
combustion of rice husk in a Torbed reactor at 750 ◦ C and 830 ◦ C, the
burnt RHA samples were further ground. The combined treatment of
RHA led to an increase in the specific surface area by 1.4 times. In
addition, on comparing RHA produced from Torbed reactor with that
from fluidised bed, the BET value was higher for the former owing to
more efficient oxidation of carbon particles (Nehdi et al., 2003).
5.2. Influence of thermomechanical treatment on pozzolanic activity
From sections 3 and 4, it is evident that the grinding duration, as well
as the burning temperature, have a significant influence on the pozzo­
lanic performance of AWAs. In this section, the combined effect of
grinding and burning on the pozzolanicity of AWAs is discussed, and the
comparison of thermally treated and thermomechanically treated AWAs
are shown in Fig. 14. While the reactivity index of unground CCA
calcined at 500 ◦ C was found to be below the minimum requirement of
75% as per ASTM C618, the pozzolanic activity index was enhanced as a
result of grinding CCA for an optimum duration of 60 min (ASTM C618,
2019). The increase in the fineness of CCA particles after grinding for 60
min was stated as the reason for the enhancement in the pozzolanic
reactivity of ground CCA. Even though the pozzolanic reactivity was
improved on further grinding, the energy required for grinding beyond
60 min was high (Memon and Khan, 2018). In a similar manner, the
direct influence of grinding on the specific surface area as well as the
reactivity of CSA was observed by Memon et al. When CSA burnt at
500 ◦ C was further ground for an optimum duration of 120 min, the
specific surface area was increased from 4960 cm2/g to 5610 cm2/g.
Therefore, the observed pozzolanic activity index and Chapelle activity
values were higher for the processed CSA sample. The PAI value was
increased from 96.8 to 108.3%. Likewise, a notable rise in the Chapelle
activity of CSA by 153.7 mg/g was witnessed in the same study (Memon
et al., 2020).
The burning of a raw SCBA sample at 700 ◦ C showed an improve­
ment in the PAI, and it was further enhanced when the burnt SCBA ash
was ground to a fineness of 300 m2/kg. However, the PAI of burnt and
ground SCBA was lower than sieved and ground SCBA. This can be
attributed to the presence of fibrous particles in the burnt and ground
SCBA. Consequently, higher water demand to maintain the same flow of
control mortar resulted in the reduction of PAI value of the burnt and
ground SCBA blended mortar (Bahurudeen and Santhanam, 2015). The
lime reactivity test as per IS:1727 was conducted by Rajasekar et al. to
evaluate the pozzolanic reactivity of SCBA burnt at various temperatures
ranging from 450 to 650 ◦ C and then ground in a vibratory ball mill for
60 min and 120 min. Among all the thermomechanically treated sam­
ples, the highest lime reactivity was reported for the SCBA burnt at
550 ◦ C for 60 min and ground for 120 min (IS:1727, 2004; Rajasekar
et al., 2018).
From Fig. 14 (a) it can be depicted that the activity index was below
75% for an unground WSA burnt at 600 ◦ C whereas, an improvement in
the pozzolanic reactivity by 58.7% was observed due to further grinding
R. Rithuparna et al.
Fig. 13. Effect of thermomechanical treatment on specific surface area compared to other processing methods: (a) BET (b) Blaine’s fineness.
Fig. 14. Effect of thermomechanical processing on pozzolanic activity compared to other processing methods: (a) PAI (b) Chapelle activity.
of the ash for 120 min. Similar results were attained for Chapelle activity
of the ground and burnt WSA sample, which increased from 450 mg/g to
520 mg/g of the pozzolan, as shown in Fig. 14 (b) (Memon et al., 2018).
The BLA subjected to combined processing methods such as burning
(bamboo leaf burnt at 500 ◦ C for 4 h), sieving and grinding showed a PAI
value of 85.97%, which is well above the minimum requirement speci­
fied by ASTM C311 (Dhinakaran and Chandana, 2016). A similar
observation was reported for RSA by Athira et al. (G. Athira et al., 2021).
Hence, better performance was exhibited when a combined processing
method was employed to obtain reactive AWAs.
5.3. Influence of thermomechanical treatment on compressive strength of
blended cementitious systems
Agro-waste ashes which were subjected to both thermal and me­
chanical treatments had higher pozzolanic performance, and a subse­
quent improvement in the compressive strength was also reported.
When CSA was calcined at 500 ◦ C and thereafter ground in a ball mill for
120 min, the strength of CSA blended concrete was increased from 25.2
to 42.2 MPa, which was even higher than control concrete (Memon
et al., 2020). A concrete with sieved, thermally treated and ground
POFA (20% replacement) exhibited a normalised compressive strength
of 1.09 with respect to control concrete (Alsubari et al., 2015).
Furthermore, for 40% replacement of cement with ultrafine POFA, the
compressive strength was 1.12 times higher than control concrete, as
shown in Fig. 15 (Zeyad et al., 2013). The filler effect and the high
pozzolanic reactivity owing to the large surface area of the fine POFA
particles are the reason for the enhancement in the strength (Alsubari
17
Journal of Cleaner Production 316 (2021) 128242
et al., 2015). Open burnt WSA, which was heat-treated at 670 ◦ C for 5 h
and further ground in a ball mill for a duration of 60 min, was used as a
pozzolan in concrete. The strength of the treated WSA blended concrete
was found to be higher than that of concrete incorporating untreated
WSA owing to the adopted thermomechanical treatment. The higher
surface area of treated WSA particles contributes to a greater number of
nucleation sites for the hydration of cement. Besides, the reduction in
the strength due to the dilution effect at higher replacement levels of
cement with WSA was reported to be insignificant for higher degrees of
grinding (Qudoos et al., 2018). Moraes et al. investigated the influence
of processed BLA in concrete. The as-received BLA was calcined at
738 ◦ C, and sieved through a 300 μm sieve. Afterwards, the sieved BLA
was ground for 50 min to obtain processed BLA. The addition of the
processed BLA as SCM (30% replacement) enhanced the compressive
strength by 56% compared to the control specimen after 90 days of
curing (Moraes et al., 2019).
For thermomechanically treated SCBA and RHA samples, there was a
significant improvement in the strength compared to the control spec­
imen (Bezerra et al., 2017; Xu et al., 2012). The amorphous nature of
silica present in the treated SCBA is the reason for the better strength.
This can be confirmed by the micrograph of the burnt and ground SCBA
samples which revealed homogenous spherical particles of size less than
10 μm (Bezerra et al., 2017). A study by Oertel et al. reported that these
spherical shaped particles were composed of amorphous silica (Oertel
et al., 2014). Jagadesh et al. studied the influence of combined grinding
and burning on the compressive strength of processed SCBA. The pro­
cessed SCBA used in the study was obtained by grinding SCBA in a ball
mill for 45 min and then calcining the ground ash in a muffle furnace at
R. Rithuparna et al. Journal of Cleaner Production 316 (2021) 128242

Fig. 15. Compressive strength of thermomechanically treated ash blended specimens.

400 ◦ C for 4 h. The compressive strength of concrete blended with 10% of the sieved SCBA blended concrete can be attributed to the larger
processed SCBA was 28% higher compared to the control concrete, particle size compared with ground SCBA. It was observed that the mean
while incorporating 10% sieved SCBA reduced the compressive strength particle size of processed SCBA was 30 μm which is much smaller than
of blended concrete by 14%. The reduction in the compressive strength the particle size of sieved SCBA (105 μm), resulting in higher strength

Fig. 16. Effect of acid treatment on BET.

18
R. Rithuparna et al.
(Jagadesh et al., 2018). Le et al. studied the properties of slag-SCBA
based ternary blended concrete. SCBA used in the study was calcined
at 800 ◦ C for 1 h. Afterwards, the calcined SCBA was further ground to
attain a fineness comparable to that of cement. The compressive strength
of the ternary blended specimen (30% slag and 30% SCBA) was found to
be as good as the control specimen (Le et al., 2018). On comparing the
strength of concrete blended with unground and ground CCA, which
were incinerated at 500 ◦ C, a significant increase in the strength was
noticed for ground CCA blended concrete. The higher surface area and
denser packing were stated as the reasons for the enhancement in
strength (Memon and Khan, 2018).
6. Chemical and thermochemical treatment
6.1. Influence of chemical treatment on specific surface area
A thermochemically treated RHA was reported to have an extremely
high specific surface area compared with thermally treated RHA, as
shown in Fig. 16. The creation of mesopores in the microstructure of the
material is responsible for the increased SSA. This can be attributed to
the leaching out of K+ ions from the potassium melt on treating the rice
husk with 1N HCl for 24 h (Salas et al., 2009). A similar increase in the
specific surface area of RHA from 90,000–235000 m2/kg was reported
when the rice husk was acid washed in 1M HCl solution before burning
at 500 ◦ C. Besides, the SSA is governed by the burning temperature of
the ash, and a reduction in the SSA was observed due to the increase in
the burning temperature from 400 ◦ C to 900 ◦ C. This can be explained by
a thermal destruction theory which states that as the degree of burning
increases, the Si–OH groups present in the silica-rich RHA will
co-condense, resulting in the collapse of the porous framework (Xiong
et al., 2009). On comparing the SSA of acid treated RHA and untreated
RHA measured by the nitrogen absorption method, the specific surface
area of RHA treated with 1N HCl showed 1.3 to 4.3 times higher SSA
than untreated RHA at burning temperatures ranging from 550 ◦ C to
700 ◦ C (Feng et al., 2004). Vayghan et al. carried out a microstructural
analysis to study the influence of acid pre-treatment on RHA. It was
observed that when acid treated and raw RHA were ground in a ball mill
with the same grinding energy, the particles of acid treated ash were
finer with a higher BET surface area compared to the raw RHA. The
increase in the specific surface area can be attributed to the leaching out
of K2O, which consequently led to an increase in the melting point of
silica. The reduction in the surface melting of silica during combustion
of the acid treated RHA helps to retain the cellular microstructure of the
RHA. As a result, it is easier to grind the treated RHA particles to smaller
sizes than the untreated RHA particles with a melted surface (Vayghan
et al., 2013).
A comparative study of different chemical treatments (acid leaching
with HCl, H2SO4 and HNO3 and boiling water leaching) revealed that
acid leaching and water leaching were effective in increasing the SSA
significantly. The acid leached RHA particles had approximately 3 times
higher SSA than untreated RHA, whereas water leached RHA particles
had 1.8 times higher SSA. The increase in the specific surface area owes
to the leaching out of alkali metals and the hydrolysis of cellulose and
lignin into smaller compounds. Further, the leaching pre-treatment also
led to the opening up of more pores in the cellular structure and resulted
in a highly porous RHA (Xu et al., 2018). A similar study of
pre-treatment of rice husk with hydrochloric acid, sulfuric acid and
acetic acid showed that the SSA of the particles was highest for H2SO4
treated RHA (63% increase compared to the untreated RHA) and lowest
for acetic acid treated RHA (only 9% increase). The HCl leached RHA
also showed a similar increase in SSA as that of H2SO4 treated RHA. An
increase in the number of mesopores after acid pre-treatment of RHA
resulted in higher nitrogen absorption and is the reason for the higher
specific surface area of treated RHA (Chen et al., 2017). The effect of
pre-treatment using HCl and H2SO4 on the SSA of RHA particles was also
studied by Bakar et al. The BET surface area of RHA treated prior to
19
Journal of Cleaner Production 316 (2021) 128242
burning at 600 ◦ C was increased by 88% and 79% for HCl and H2SO4
leached RHA, respectively. The hydrolysis of organic compounds pre­
sent in RHA into smaller compounds, which are easier to decompose
during the calcination was stated as the reason for the increase in SSA of
RHA particles (Bakar et al., 2016).
Saad et al. studied the influence of pre-treating rice husk in 0.1N HCl
for three soaking durations (1 h, 2 h and 3 h). The acid treated rice husk
was then burnt at 700 ◦ C and 800 ◦ C for 1 h and later ground in a ball
mill for 1 h to obtain ultrafine RHA. The particle size analysis showed
that the mean particle size was smallest for RHA soaked for 3 h in HCl,
which is 4.5 μm and small particle size implies larger SSA (Saad et al.,
2016). Pre-treatment of SCSA with HCl and hot deionised water has led
to a significant increase in the BET surface area of the SCSA particles.
The extremely high fineness of the acid treated SCSA was attributed to
the highly porous structure of the ash after acid leaching, as depicted in
the micrograph of the acid treated SCSA. The BET surface area of acid
leached SCSA was reported to be 10 times higher than untreated SCSA,
while it was 1.5 times higher for water leached SCSA (Cordeiro et al.,
2017). In the same way, soaking of sugarcane bagasse in 0.1M HCl led to
a notable increase in the SSA up to 5 times higher than untreated ash
owing to the higher number of microvoids formed in the porous struc­
ture of the pre-treated ash (Embong et al., 2016). In another study,
elephant grass ash (EGA) pre-treated in 1N HCl solution and washed in
hot deionised water were compared, and the BET value was found to be
64% higher for acid leached sample (Cordeiro and Sales, 2015). Acid
treated RSA and WSA also exhibited similar improvement in the surface
area by 11.83 times and 6.08 times, respectively, when compared with
the untreated samples. Pre-treatment of ashes with sulfuric acid led to
the removal of phosphorous and potassium ions from the ashes. This
aided in enhancing the reactivity of the treated ashes as the absence of
these ions increased their SSA (Ataie and Riding, 2013). Moreover, the
BET surface area of acid treated RSA burnt at 500 ◦ C was reported to be
20 times larger than silica fume owing to the higher internal porosity of
RSA (Ataie and Riding, 2016). Similarly, acid leaching of corn straw
with 0.52M citric acid for 48 h prior to the burning significantly reduced
the K+ ion concentration in CSA from 17.2% to 0.3%. A corresponding
increase in the BET surface area of CSA from 13320 to 171690 m2/kg
was also witnessed in the study (de Lima and Cordeiro, 2021).
6.2. Influence of chemical treatment on LOI
The influence of acid treatment on the carbon content of AWAs is
shown in Fig. 17. For acid-treated RSA as well as WSA, there was a
significant reduction in the LOI. A direct correlation between the metal
oxides content in the ash and LOI was noted. Moreover, on comparing
pre-treated RSA and WSA, the LOI was lower for RSA, owing to a lower
alkali content in the rice straw compared to the wheat straw (Ataie and
Riding, 2013). The removal of cellulose and lignin when the corn stalk
was soaked in a 0.1M diluted HNO3 solution before the burning process
was stated to help in removing the organic matter during the calcination
of the corn stalk (Shakouri et al., 2020). The LOI of CSA was found to be
decreased from 9.04% to 0.16%, as the K2O content reduced from 22.7%
to 0.94% (Shakouri et al., 2020). It was stated that during the burning of
agro-waste based biomass in cogeneration boilers, potassium oxides
(K2O) start to dissociate at a temperature above 350 ◦ C. During the
decomposition of alkali metal oxides like K2O, the surface melt is
formed. Carbon from organic matters like lignin and cellulose will be
trapped in the melt formed and thereby results in high LOI. Hence, the
removal of alkali oxides using pre-treatment could help in the removal of
organic content. Therefore, a direct correlation between the alkali metal
oxides content in the ash and the LOI exists (Krishnarao et al., 2001). For
that reason, acid treated CSA in Fig. 17 has less LOI. The presence of K2O
was also reported to accelerate the surface melting of silica particles in
RHA. The low melting point silicates are formed by the reaction of K2O
with SiO2 during the combustion of rice husk. This prevents the volati­
lisation of organic matter and results in higher unburnt carbon content
R. Rithuparna et al. Journal of Cleaner Production 316 (2021) 128242

Fig. 17. Comparison of LOI for acid-treated and untreated samples.

in the RHA. Hence, the LOI of acid leached RHA will be higher than raw acid. It was reported that acid pre-treatment of these ashes caused the
RHA due to the removal of K2O from the rice husk (Chen et al., 2017; removal of crystalline phases from the ashes (Ataie and Riding, 2014b).
Vayghan et al., 2013). On comparing the unburnt carbon content in The leaching out of alkalis such as K2O and Na2O when the ashes are
untreated RHA and CSA, it was observed that the LOI was higher for acid pre-treated can be stated as the reason for higher amounts of
untreated CSA (4%) compared to the untreated RHA (3.3%). However, amorphous silica in the treated ashes. This is because the presence of
after pre-treating the CSA with 0.52M citric acid for 48 h, the LOI was alkalis in the ash will otherwise accelerate the formation of crystalline
decreased to 2.3% (de Lima and Cordeiro, 2021). Another study showed silica during the calcination of the agro-waste (Vayghan et al., 2013).
that pre-treatment with inorganic acids such as HCl and H2SO4 was more Therefore, prior treatment of agricultural residues using acids before
effective in the removal of K+ ions (98–100%) than organic acids such as burning can significantly improve the pozzolanic reactivity, as shown in
acetic acid (91%) (Chen et al., 2017). A similar reduction in LOI of SCBA Fig. 18. Acid pre-treatment of sugarcane bagasse for a soaking period of
after rinsing with acids was observed. The leaching out of alkali metals 1 h in 0.1M HCl was recommended as optimum by Embong et al. SCBA
caused better burning of bagasse in the cogeneration boiler. Further­ treated using optimal concentration showed improved pozzolanic
more, the structural changes in cellulose and lignin caused by acid reactivity by 70% compared to the untreated ash. Soaking in low
treatment helped in the removal of carbon rich fibrous particles avail­ concentrated acid facilitated the removal of lignocellulosic compounds
able in bagasse during the calcination process and hence reduced the
LOI (Ataie and Riding, 2014a; Embong et al., 2016).
Two pre-treatment methods, namely, hot ionised water washing and
acid leaching, were employed by Cordeiro et al. to reduce the metallic
oxides and carbon content present in sugarcane straw. Both the methods
significantly reduced the LOI content in the ash and led to better silica
purification. Furthermore, the acid leaching was reported to be more
effective in the dissolution of K2O, SO3 and CaO, which is evident by the
low LOI value of 1.2% in the acid leached SCSA sample. The white
colour of the acid-treated ash as compared to the light grey colour of the
raw SCSA confirms this observation (Cordeiro et al., 2017). The acid
treatment of elephant grass prior to the burning also resulted in lowering
of LOI of elephant grass ash by 69% (Cordeiro and Sales, 2015).

6.3. Influence of chemical treatment on pozzolanic reactivity

The prior treatment with acid was not only effective in reducing the
carbon content but also helped in the transformation of silica present in
the material to amorphous form. This can be confirmed by comparing
the XRD patterns of raw and treated SCSA, which revealed that peaks of
quartz present in the diffraction pattern of raw ash were not detected in
that of the treated ash (Cordeiro et al., 2017). Similar observations were Fig. 18. Comparison of Chapelle activity of acid-treated and un­
also witnessed in the case of CSA, WSA, and RSA treated with sulfuric treated samples.

20
R. Rithuparna et al.
present in the bagasse and assisted in extracting a higher amount of
silica (Embong et al., 2016). The soaking of palm oil clinker powder in a
solution with different concentration of HCl revealed that the Chapelle
activity was highest (by 118%) for POFA pre-treated with 0.5M HCl.
Furthermore, the pozzolanic reactivity was found to reduce by
increasing the acid concentration from 0.5M to 1M (Ismail 2020). The
enhancement of solubility of cellulose and hemicellulose on treating
with higher acid concentration led to the elimination of amorphous
cellulose fraction. This resulted in the accelerated crystallisation of silica
during the combustion process, thereby lowering the pozzolanic reac­
tivity of AWAs (Embong et al., 2016). An increase in the Chapelle ac­
tivity from 883 to 998 mg/g of CaO was reported on treating elephant
grass in 1N HCl for 2 h before the burning. This increase can be attrib­
uted to the availability of a greater surface area for the pozzolanic re­
action (Cordeiro and Sales, 2015).
The conductivity method proposed by Luxan et al. is a rapid method
for evaluating the pozzolanic reactivity of agro-waste ashes. A greater
change in the conductivity of pozzolan-saturated lime solution indicates
a higher pozzolanic reactivity. For a material to be a good pozzolan, the
change in conductivity of the solution should be greater than 1.2 mS/
cm. If the change in the conductivity is between 0.4 and 1.2, the material
falls under the category of variable pozzolanicity, and if the value is less
than 0.4, then it is a poor pozzolanic material (Luxan et al., 1989). This
method was also employed by Feng et al. to compare the pozzolanic
reactivity of HCl treated RHA, and untreated RHA produced at different
burning temperatures. The results showed that the change in conduc­
tivity of saturated lime solution with treated RHA was higher than that
with untreated RHA at temperatures ranging from 350 to 1000 ◦ C.
Further, it was observed that untreated RHA showed good pozzolanic
reactivity up to a burning temperature of 750 ◦ C whereas pre-treated
RHA had better reactivity up to 1000 ◦ C. The larger specific surface
area of RHA particles and greater amount of amorphous silica in the acid
treated RHA was stated as the reason for the higher pozzolanic reactivity
(Feng et al., 2004). The presence of amorphous silica in the acid treated
RHA is confirmed by the smooth broad peaks and absence of cristobalite
peak (2θ ≈ 22◦ ) in the X-ray diffractogram (Chen et al., 2017). The
conductivity change test was performed by Xu et al. for RHA pre-treated
with different chemicals such as HCl, H2SO4, HNO3 and boiling water.
The change in the conductivity was observed to be 6.09, 5.73, and 5.91
for HCl, H2SO4, and HNO3 leached RHA, whereas, for boiling water
leached RHA, the conductivity change was 4.42. All these values were
approximately 10 times higher than that of untreated RHA. Even though
it is evident that acid pre-treatment has a more significant influence on
the pozzolanic reactivity of RHA, the water leaching treatment method
is more economical. The effect of acid leaching on the temperature
dependence of crystalline silica formation was studied using the X-ray
diffraction technique. The XRD patterns of acid treated RHA burnt at
various temperatures confirmed that silica in RHA remained amorphous
even after burning RHA at a temperature of 900 ◦ C for 6 h. This can be
attributed to the leaching out of alkalis which would have otherwise
reacted with silica present in RHA to form a compound with low crys­
tallisation temperature (Xu et al., 2018).
Cordeiro et al. evaluated the pozzolanic reactivity of SCSA treated
with hot deionised water leaching and acid leaching (1M HCl, 2 h) using
the conductivity method proposed by Luxan et al. The variation in
conductivity of untreated SCSA was 1.07 mS/cm, whereas for water
leached and acid leached SCSA, it was 2.89 and 5.8 mS/cm, respectively.
Even though untreated SCSA falls under the category of poor pozzola­
nicity, both the treated SCSA are classified as a good pozzolanic mate­
rial. The better pozzolanic reactivity of acid leached SCSA was
confirmed by the modified Chapelle test, which showed 24% higher
reactivity when the SCSA was acid leached prior to the burning. This can
be attributed to the presence of higher amorphous silica, and lower
unburnt carbon content in acid leached SCSA (Cordeiro et al., 2017).
Similarly, acid treated CSA (0.52 M citric acid for 48 h) was also clas­
sified as a good pozzolan owing to a high electrical conductivity
21
Journal of Cleaner Production 316 (2021) 128242
variation of 5.83 mS/cm which is greater than 1.2 mS/cm (de Lima and
Cordeiro, 2021). The conductivity change method was performed to
compare the pozzolanic reactivity of three AWAs pre-treated with citric
acid and then subjected to conjugate burning (in a pilot kiln and after­
wards in a muffle furnace at 600 ◦ C). The variation in the electric con­
ductivity was found to be 5.78, 3.73, and 5.91 mS/cm for RHA, CSA and
BLA, respectively (Cordeiro et al., 2020). These values indicate that all
the ashes fall under the category of a good pozzolanic material as per the
criteria (Luxan et al., 1989).
6.4. Influence of chemical treatment on compressive strength of blended
cementitious system
The several studies conducted on concrete blended with processed
AWAs revealed that chemical treatment before burning of the agricul­
tural residues has a significant influence on the compressive strength of
concrete. A comparison of normalised compressive strength of concrete
blended with untreated and treated residual ashes with respect to the
control concrete is presented in Fig. 19. On comparing thermally treated
and thermochemically treated RHA incorporated concrete, the
compressive strength was increased by 1.05 and 1.17 times that of OPC
concrete, respectively. The enhanced strength for concrete mixed with
thermochemically treated RHA can be attributed to the higher reactivity
of treated ash and better pore refinement (Salas et al., 2009). The
compressive strength of cement mortar blended with acid treated RHA
was reported to be improved by 7.6% and 12% compared to untreated
RHA blended cement mortar at 28 days and 91 days of curing, respec­
tively. The higher strength of treated RHA can be attributed to the
higher pozzolanic reactivity due to the larger specific surface area and
higher reactive silica content (Feng et al., 2004). A similar result was
obtained for RHA treated with 0.1M HCl for 90 min prior to the burning
at 700 ◦ C. The compressive strength of RHA blended paste (10%
replacement) after 28 days of curing was found to be 31.68 MPa, and
33.79 MPa for raw and acid treated RHA, respectively (Liu et al., 2020).
Vayghan et al. also stated enhancement in the compressive strength of
the RHA blended concrete when the ash was treated with 0.01N HCl for
1 h prior to the burning (Vayghan et al., 2013). On comparing acid
leaching and water leaching pre-treatment methods for RHA, it was
observed that the compressive strength of acid treated RHA blended
paste (67.4 MPa) was 48.1% higher than the control paste, whereas
water leached RHA blended paste had 42.4% higher strength. Further­
more, it was reported that the duration of water leaching of rice husk
had minimal effect on enhancing the reactivity of treated RHA (Xu et al.,
2018). In another study, the 28-day compressive strength of a mortar
blended with 15% RHA (soaked in 5M HCl for 7 days and then burnt at
600 ◦ C for 2 h) was reported to be slightly higher than that of a mortar
blended with 15% silica fume. The enhanced strength of the former
owes to the higher pozzolanic reactivity of acid treated RHA compared
to silica fume (Hu et al., 2020).
An improvement in the compressive strength from 23.5 MPa (raw
SCBA blended concrete) to 26 MPa (acid-treated SCBA blended con­
crete) was observed when sugarcane bagasse was soaked in 0.1M HCl for
1 h before calcination. The substantial reduction in K2O on treating
sugarcane bagasse with HCl reduced the possibility of crystallisation of
silica at a lower temperature. The Chapelle activity test performed in the
same study confirmed the enhancement in the pozzolanic reactivity of
treated SCBA compared to the untreated ash (Embong et al., 2016). The
influence of acid treatment prior to the burning of other agro-wastes
such as wheat straw, rice straw and corn stalk is also studied in
various literature. The compressive strength of the specimen incorpo­
rating untreated WSA and CSA was found to be lower than the control
specimen, as shown in Fig. 19. However, prior treatment with acid
before the burning of wheat straw and corn stalk led to a substantial
increase in the compressive strength of respective blended concrete
owing to the improved pozzolanic reactivity (Ataie and Riding, 2013;
Shakouri et al., 2020). Similarly, the compressive strength of mortar
R. Rithuparna et al.
Fig. 19. Normalised strength for acid-treated (AT) and untreated ash blended specimens.
blended with pre-treated CSA (0.52M citric acid for 48 h) was found to
be 42% higher than untreated CSA blended mortar. The increase in
fineness and the pozzolanic reactivity of CSA was stated as the reason for
the improvement in the strength of the mortar (de Lima and Cordeiro,
2021). A reduction in the portlandite content and an increase in the
strength of mortar by 32% were reported due to the addition of RSA
(obtained from rice straw pre-treated with HCl for 24 h) when compared
with mortar containing untreated RSA. The acid treatment was found to
be effective in removing alkali metals and other impurities from the rice
straw. This led to a larger internal surface area and higher content of
amorphous silica in the residual ashes (Ataie and Riding, 2013).
7. Discussion
7.1. Optimum processing conditions for different AWAs
From the detailed and comprehensive review, it can be stated that
processed AWAs have a very good advantage over raw ashes owing to
their superior performance when blended with cement. The main
disadvantage of utilising raw ashes without any prior treatment is the
high amount of unburnt carbon content and low pozzolanic reactivity.
The temperature at which the agricultural residues are burnt plays a
crucial role in deciding the amount of unburnt carbon and the amor­
phous silica content in the residual ashes. For maximising the reactivity
of a material, it ought to be burnt at an optimum temperature to attain a
minimum amount of residual carbon and maximum amorphous silica
content. The open field burning of the agro-waste residues in uncon­
trolled conditions result in the low reactivity of the residual ashes. In
some cases, even the AWAs obtained from the controlled burning
exhibited poor performance owing to the large particle size and lower
specific surface area of residual ashes. Therefore, the need for further
processing of the materials before using them as supplementary
cementitious materials is of utmost importance.
22
Journal of Cleaner Production 316 (2021) 128242
It is imperative to note that the method of pre-treatment to be
adopted must vary with respect to the type of AWAs. For instance, RHA
burnt at an optimum temperature in the range of 500–650 ◦ C had a
pozzolanic reactivity of 95%, whereas on burning the corn cob at 500 ◦ C,
the activity index was below the minimum requirement (75%) as per
ASTM C618. When the CCA obtained was further ground to a particle
size of 29 μm, the PAI value was found to be increased from 53.7% to
77.6%, as shown in Fig. 20. In a similar manner, the pozzolanic reac­
tivity of WSA was improved from 62.2% to 98.7% on comparing the
thermomechanically treated sample with the thermally treated sample.
However, sieving and grinding of SCBA to a fineness of 45 μm resulted in
the higher pozzolanic activity when compared to thermomechanical
treatment (burnt and ground) of SCBA. Similarly, it can be noted that the
grinding of raw RHA was sufficient to enhance the properties of the ash.
Grinding of the ashes will mainly influence the particle size and specific
surface area of the ashes. An increase in the surface area will result in the
availability of a greater number of nucleation sites for the pozzolanic
reaction to take place. In order to improve the pozzolanic reactivity
further, the agro waste can be treated with chemicals before the burning
process. Several studies reported the presence of a high amount of alkali
metals and impurities in the agricultural residues. The alkali metals will
trap the carbon present in the agro-waste during its burning. Acid
treatment was found to be effective in promoting the leaching of the
impurities such as K2O and other alkali metals, which will otherwise
hinder the removal of carbon and volatile matter during the burning
process. Soaking the material in acid solutions also result in the breaking
down of lignin and decrystallisation of cellulose available in the mate­
rial. The surface area of acid-treated RSA was enhanced by 11.83 times
compared to the untreated RSA, and it resulted in 32% increase in the
compressive strength of blended mortar.
It is clearly evident from the study that different levels of pozzolanic
performance of the treated AWA can be achieved based on the method
and degree of pre-treatment adopted. Some of the AWAs such as CCA,
R. Rithuparna et al.
Fig. 20. Optimum parameters for processing of different materials.
CSA and WSA exhibited higher pozzolanic reactivity when these ashes
were ground after burning at their respective optimum temperatures.
However, studies were limited to the processing of these agro-wastes
such as rice straw, elephant grass, maize stalk etc. Therefore, it is
necessary to study the influence of different processing methods on their
reactivity to enable their acceptance as an SCM. At the same time, a lot
of research studies attempted on the processing of RHA and SCBA.
Moreover, only grinding for an optimum duration was suggested to
attain adequate pozzolanic performance of RHA and SCBA. Another
added advantage of pre-treating the AWAs is the possibility of higher
replacement of cement when the concrete is incorporated with these
ashes. Therefore, the cement manufacturer has to opt for the necessary
processing methods to achieve the performance expected from the
concrete blended with the treated material. Understanding the appro­
priate processing technique for the AWAs will lead to a higher accep­
tance of these materials in the cement industry.
Fig. 21. Schematic diagram of the reaction mechanism.
23
Journal of Cleaner Production 316 (2021) 128242
7.2. Reaction mechanism of processed AWAs
Mechanical and durability properties of the blended cementitious
system are enhanced by the addition of AWAs as a result of the pozzo­
lanic reaction. The pozzolanic reaction involves the reaction between
silica in AWAs and the portlandite to form calcium silicate hydrate
(CSH), thereby improving the properties of blended systems. The rate of
the pozzolanic reaction is significantly governed by different methods
adopted for processing the AWAs. Villar-Cocina et al. studied the reac­
tion mechanism between silica in AWA and calcium hydroxide using
decreasing nucleus model. As per this model, AWAs are considered as
spherical particles. In an AWA-lime solution mixture, initially, Ca2+ ions
are diffused from the lime solution. Afterwards, Ca2+ ions are absorbed
by the surface of the spherical AWA particles. The radius of unreacted
AWA (r) is found to decrease as the absorbed Ca2+ reacts with the AWA
to form CSH (as depicted in Fig. 21). At the later stage of the reaction,
the Ca2+ ions need to further penetrate through the initially formed
products in the outer layer of the AWAs (Villar-Cociña et al., 2003). As
the reaction progresses, the thickness of reaction products (x) increases.
R. Rithuparna et al.
Moreover, LOI, specific surface area, particle size and chemical
composition of AWA are the key factors which influence this reaction
mechanism. The processing methods such as burning, grinding, sieving
and chemical treatment modifies the above mentioned key factors and
hence, alter the reaction rate.
The burning of agro-waste ashes causes significant changes in their
properties. Agricultural biomass mainly consists of cellulose, hemicel­
lulose, lignin and moisture content. Due to burning, these biomasses are
converted majorly to silicon dioxide and other oxides. The higher pro­
portion of silica qualifies these biomass ashes to be used as cement
replacement material. In the microstructural analysis of AWA, silica is
found to be mainly accumulated in the phytoliths. Sintering and fusing
of these phytoliths occur at higher temperature. Moreover, from the XRD
analysis, as the burning temperature increases, the nature of silica
changes from amorphous to crystalline (Athira et al., 2021). Crystal­
lisation of silica reduces the pozzolanic reactivity of the agro-waste
ashes. Furthermore, the volatilisation of organic matter increases as
the burning temperature increases. Therefore, reduction in organic
fraction leads to the reduction of LOI, which also adds to the increase in
the reactivity of the ashes. However, some fraction of agro-waste ashes is
witnessed as unburnt particles after calcination, and it is the reason for
marginally high LOI value for AWAs compared with industrial
by-products such as slag and fly ash.
Grinding and sieving are two physical treatment methods adopted
for agro-waste ashes. Sieving helps to remove coarser particles. Gener­
ally, coarse fibre particles are carbon rich unburnt fraction of AWAs,
which in turn imparts a higher LOI value. Hence, sieving helps to
separate these fibrous particles, and subsequently, a reduction of LOI
can be attained. Furthermore, the grinding improves the specific surface
area of agro-waste ashes. As a result, the reactivity of ground ashes in­
creases. However, increasing fineness causes a rise in the water demand
for most of the agro-waste ashes. On the contrary, excess grinding of
RHA leads to the collapse of its cellular structure and decreases the
water demand (Tuan et al., 2011). Breakdown of fibrous structures was
clearly evident at the microstructural level studied using SEM analysis of
SCBA and RHA before and after grinding. Incorporation of finer
agro-waste ashes as supplementary cementitious materials improve the
strength due to the combined result of chemical effect (pozzolanic re­
action) and physical effect (filler effect) (Jittin et al., 2020; Mohan et al.,
2021).
Another pre-treatment method for agro-waste ashes is chemical
treatment. Soaking in acid or rinsing with acids such as hydrochloric
acid, sulfuric acid, and nitric acid for a certain duration are adopted as a
chemical treatment prior to burning and has a significant influence on
the pozzolanic performance of residual ashes. Chemical treatment pre­
dominantly helps in the removal of alkali metals from biomass. More­
over, the breakdown of cellulose is also an advantage of chemical pre-
treatment. As a result of the removal of alkali metal ions, the organic
fraction is reduced on the burning of biomass. Hence, agro-waste ashes
obtained after chemical pre-treatment of biomass improved the perfor­
mance of the blended cementitious system.
7.3. Environmental footprint associated with processing of AWAs
Even though a high quantity of agricultural wastes is burnt as
biomass in a cogeneration plant, the reuse of residual ashes is minimal,
and a major quantity of ashes is disposed of as waste. The processing of
raw agro-waste ashes for their reuse requires a lot of energy and also
contributes to additional CO2 emission. Yin et al. studied life cycle
analysis with the main focus on the reuse of ago-waste ashes in cement
industries and reported sustainability aspects of agro-waste blends
attributable to a significant reduction in landfill and greenhouse gas
emission. The feasibility of incorporating agro-waste ashes in the cement
industry is not only governed by mechanical and durability character­
istics of agro-waste blended concrete, but community, technology,
transportation, commercial feasibility are also crucial parameters (Yin
24
Journal of Cleaner Production 316 (2021) 128242
et al., 2018). Furthermore, selecting an ideal processing condition is
significantly governed by the environmental footprint associated with
that processing method in addition to the improvement in the charac­
teristics of processed agro-waste ashes. Processes such as burning,
grinding, and chemical treatment increase the environmental impact.
Hence, it is necessary to balance between the impact associated with the
processing of ashes and cement clinker production to attain sustain­
ability through cement replacement with AWAs. Agro-waste ashes are
generally ground to cement fineness or lesser to obtain adequate reac­
tivity, however grinding is an energy-intensive and expensive process
(Bahri et al., 2018). RHA was ground by Kameshwar et al. using a ball
mill for 30 min, and ground RHA had D50 and BET surface area of 4.5
μm and 56.5 m2/g, respectively. The reduction in D50 and increase in
BET surface area were found to be marginal on grinding beyond 30 min.
Moreover, PAI was also increased from 82% to 93% on grinding RHA for
about 30 min with an energy requirement of 1258 kJ. Even though the
energy required to grind RHA for 120 min was 5035 kJ, the enhance­
ment in reactivity was minimal. Therefore, optimum grinding duration
is imperative to produce agro-waste ash-based sustainable blended
cement (Kameshwar et al., 2020). Moreover, on comparing the life cycle
assessment of RHA blended concrete with the respective control con­
crete, even including the high transportation cost of RHA, the RHA
blended concrete has a 28% lesser global warming potential than the
control concrete. Hence, the utilisation of RHA can significantly lower
the environmental impact of conventional concrete production (Mar­
chetti, 2020). It was reported that the cost per m3 of concrete with 20%
RHA decreased by 6% for M30 grade concrete (Moulick, 2015).
Cordeiro et al. calculated the specific grinding energy using Bond’s
law, considering the dry grinding condition in a ball mill and open cir­
cuit operation. Grinding time is directly related to energy consumption.
For instance, 60 min of grinding is required to obtain SCBA with a D80 of
15 μm. In the same study, the energy consumption for the grinding of
SCBA (D80 of 15 μm) in an industrial scale was measured and reported
as 245 kWh/t (based on the assumption that specific energy consump­
tion was 36 kWh/t). Moreover, it is imperative to note that high grinding
energy is needed for further grinding, for example, to reduce D80 from
15 to 4 μm, 240 min grinding is required, which is uneconomical. This
increase in grinding time escalates the energy consumption to approxi­
mately 800 kWh/t (Cordeiro et al., 2004). Cordeiro et al. reported the
requirement of at least 50 kWh/t of grinding power to achieve a particle
size in order to maintain PAI of SCBA greater than the minimum
permissible value of 75%. However, in the case of closed circuit grinding
operation, the energy required can be reduced to 45 kWh/t. Moreover,
300 kWh/t and 250 kWh/t of grinding power are required to achieve
PAI of 100% for open and closed circuit, correspondingly. The energy
required to achieve a PAI of 75% is only half of the electrical energy
(110 kWh/t) required for the production of ordinary Portland cement
(Cordeiro et al., 2009c). It was reported that the application of SCBA as a
supplementary cementitious material leads to a notable reduction of
519.3 kT of CO2 compared to ordinary Portland cement (Fairbairn et al.,
2010). Athira et al. reported that the utilisation of agro-waste ashes
(SCBA) available in the proximity of cement plants could reduce carbon
footprint by about 3000 tonnes per year (Athira et al., 2020).
8. Scope for future research
• Most of the earlier research studies focused on the conventional
methods of grinding and thermal processing of agro-wastes. Inves­
tigation of other effective means of pre-treatment methods is mini­
mal even though such treatment methods have proven to be
sufficient for certain materials. For instance, acid leaching and
washing the agricultural residues with hot deionised water prior to
the burning proved to be effective in improving the pozzolanic
reactivity of sugarcane straw ash and elephant grass ash. Hence, such
methods should be further explored in addition to the conventional
R. Rithuparna et al.
methods for the effective utilisation of AWAs as supplementary
cementitious materials.
• Based on the thorough review, only limited research studies reported
the influence of prior treatment methods of AWAs on the long-term
properties of blended concrete. Most of the studies were focused
on the fresh and mechanical properties of the concrete incorporated
with treated ashes. It can be noticed that the durability parameters
which were studied are resistance to chloride penetration and water
absorption capacity of treated RHA and POFA incorporated concrete.
Research studies on other long-term characteristics such as sulfate
attack, carbonation, acid attack, and shrinkage are lacking in the
literature. Furthermore, studies on the influence of other processed
agro-wastes such as SCBA, CCA, RSA, CSA and WSA on the durability
of blended concrete is also deficient. Considering the durability of
concrete as one of the major factors which govern the performance of
concrete structures in the long-term, further research must be
focused on the durability characteristics of agro-waste ashes blended
concrete.
• The fresh properties such as slump and slump flow of AWA blended
cementitious mixture is widely reported in the literature. However,
detailed studies on the rheological characteristics of AWA blends are
limited. Hence, future research on rheological properties should be
encouraged with more emphasis on the selection and compatibility
of superplasticiser and their dosage optimisation with respect to
different AWAs.
• Predominantly, many studies revolved around the processing of RHA
and SCBA. Only a few researcher studies have explored the influence
of pre-treatment on the characteristics of other residual ashes,
namely, POFA, CCA, RSA, EGA, BLA and WSA. These studies
revealed that adopting different methods of pre-treatment for agro-
wastes can improve the performance of agro-waste ashes blended
concrete. However, the lack of knowledge in this aspect is found to
hinder the acceptance of several other AWAs, which after proper
treatment could be categorised as a good pozzolan. Hence, studies in
this direction will encourage the reutilisation of several agricultural
by-products in addition to RHA and SCBA, which are the most
commonly recognised agro-waste based pozzolans. Thereby, it will
aid in reducing the carbon footprint associated with open field
burning of agricultural residues and conventional cement
production.
• From the detailed review, it is interesting to note that the method
and extent of pre-treatments required for different materials are not
the same. Moreover, the degree of processing adopted will govern
the pozzolanic reactivity of the AWAs. For instance, CCA burnt at
500 ◦ C for 30 min had an activity index of 53.7%, whereas, on further
grinding, the PAI value was increased to 77.6%. Hence, a
performance-based processing scheme should be developed for each
AWA with a detailed report of the method and level of pre-treatment
essential to meet the reactivity requirement for satisfying a specific
purpose.
• Another point to be noted is that the variation in the quality of ash
permitted for various construction products is influenced by the
intended purpose of use. The quality control of AWAs for use in
concrete will be entirely diverse from the quality control required for
use in brick manufacturing. In a similar manner, the level of pre-
treatment required for high-performance concrete will be higher
compared to conventional concrete. Therefore, a guideline should be
developed to categorise the AWAs based on the degree and the
method of pre-treatment required with respect to their usage in
different construction products. This will guarantee a significant
reduction in the needless energy consumption for processing the
materials and leads to more economical production of the AWA
blended cement.
• The conventional processing techniques for agricultural residues are
mainly energy-intensive processes. Even though these techniques are
beneficial in the aspect of performance of the blended concrete, the
25
Journal of Cleaner Production 316 (2021) 128242
adaptation of the treated materials in the industry depends on the
cost incurred for the processing. Studies that emphasize cost-
effectiveness in terms of the energy requirement of different pre-
treatment processes are highly limited. Reducing the power con­
sumption for processing the agro-waste based pozzolans leads to a
lower production cost and results in environment-friendly
manufacturing of the blended concrete. For this reason, it is imper­
ative to employ processing methods which provide a balance be­
tween energy consumption and the performance of processed AWA
blended concrete. Comparative cost analysis should be performed to
understand the economic benefit of one processing method over
another.
• Based on the previous studies, it can be concluded that the properties
of the ashes vary according to the source from which the ashes were
collected. Consequently, the method of pre-treatment to be adopted
for the same material from different sources will be dissimilar. In
order to bring about a uniform characteristic for each material,
quality control measures should be carried out while burning the
agricultural residue as biomass at the source level itself. Hence, the
production of residual ashes under controlled burning should be
promoted. A monitoring system can be developed to ensure good
quality AWAs and these value-added products can be considered as
an additional source of income for the farmers. Moreover, the
requirement for further treatment of ash before utilising in the
cementitious system can be reduced.
• According to the earlier studies, it is evident that literature is majorly
focused on the effect of different degree of processing methods on the
performance of agro-waste ash blended cementitious systems. The
replacement of cement with treated agro-waste ashes is focused to
reduce the environmental impact by reducing conventional cement
clinker production. Hence, the environmental footprint associated
with cement clinker can be cut-down to a great extent. However,
processing methods such as grinding, burning and chemical treat­
ments have an impact on environmental safety because these
methods are energy-intensive. Therefore, it is necessary to evaluate
the environmental impact and safety of the different processing
methods suggested for agro-waste ashes. Thus, a detailed environ­
mental impact assessment with respect to processing methods of
agro-waste ashes is recommended for future research.
9. Conclusions
Different methods of processing adopted for agro-waste ashes and
their influence on the properties of concrete are comprehensively
reviewed. An in-depth analysis of earlier studies has revealed that the
processing method to be adopted will vary depending on the material
under consideration and the source from which the residues were ob­
tained. The pozzolanic reactivity of material also varies according to the
method and degree of pre-treatment adopted. The salient conclusions
based on the methodical and comprehensive review are listed below.
• Grinding of agro-waste ashes resulted in a reduction of particle size
and an increase in the specific surface area of the particles. Hence,
the grinding enhances the pozzolanic reactivity of the material
owing to the availability of a greater number of nucleation sites for
the reaction to take place.
• Grinding of RHA and SCBA for the respective optimum duration is
sufficient to improve their pozzolanic performance. Further increase
in the grinding duration beyond their optimum grinding times leads
to only a marginal increase in the reactivity.
• The residual agro-waste ashes obtained by open-field burning of the
agro-wastes exhibited low activity index and high carbon content
compared to processed ashes.
• The studies related to thermal treatment of residues indicated that
good quality ash could be obtained only when the residues are
incinerated at an optimum temperature for an optimal duration.
R. Rithuparna et al.
Based on the review, the optimum temperature of RHA, SCBA, POFA,
WSA and CCA are 600 ◦ C, 700 ◦ C, 500 ◦ C, 600 ◦ C and 500 ◦ C,
respectively.
• Reduction of pozzolanic reactivity is witnessed at lower as well as at
extremely higher temperatures. The higher amount of residual car­
bon at a lower temperature due to incomplete burning and the
crystallisation of silica at higher temperature led to lower reactivity.
• Thermomechanical treatment results in better performance
compared to only thermal treatment for certain agro-ashes such as
CCA, CSA and WSA. The enhancement in pozzolanic reactivity is
attributed to the larger specific surface area and higher content of
amorphous silica when the control burnt ash is further ground for its
optimum grinding time.
• Chemical treatment of agro-wastes prior to burning showed great
improvement in the chemical characteristics of residual ashes. One of
the limitations of utilising agro-wastes is the presence of alkali metals
such as potassium in the material. The K+ ion will trap carbon and
other volatile matter from burning off due to the formation of a layer
of alkali melt over the surface. The treating with deionised water and
acids caused the leaching of the alkali metals and resulted in better
removal of residual carbon. Hence, the chemical treatment enhances
the pozzolanic reactivity of agro-ashes.
• Significant improvement in the strength and durability properties of
processed agro-waste blended concrete is evidently witnessed. The
increase in the strength of agro-waste ash blended concrete
compared to control concrete is in the range of 10–60%, 10–25% and
11–50%, respectively, for grinding, controlled burning and acid
treatments.
The utilisation of processed agro-waste ashes in the cement industry
will have multiple advantages. The availability of good quality ash with
uniform characteristics and high strength of concrete blended with
treated ash will lead to better acceptance of the agro-wastes in the
cement industry. Secondly, reutilisation of agricultural residues will be
an effective way of waste management and thereby, it reduces the
environmental impact caused by their disposal or open-field burning of
agricultural residues.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
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