Waste and Biomass Valorization (2020) 11:1627–1634

https://doi.org/10.1007/s12649-018-00556-y

ORIGINAL PAPER

A Comparative Study on the Pozzolanic Activity Between Bamboo

Leaves Ash and Silica Fume: Kinetic Parameters
Ernesto Villar‑Cociña1 · Loic Rodier2 · Holmer Savastano Jr2 · Manuel Lefrán1 · Moisés Frías Rojas3

Received: 17 September 2018 / Accepted: 17 December 2018 / Published online: 2 January 2019
© Springer Nature B.V. 2019

Abstract
Silica fume is the most performing siliceous product among the pozzolanic materials. This is mainly related to his high
content (around of 90%) of amorphous silica. However, this residue has a high cost and the quantities available are limited.
This limits its use in the modern construction industry, particularly in developing countries. For this reason it is motivating to
look for an alternative to replace it with other waste materials with similar behavior, especially in these countries. It is known
that bamboo leaf ash (BLAsh) is a pozzolan with high reactivity, possessing a high amount of amorphous silica. The paper
presents a qualitative and quantitative characterization of the pozzolanic reactivity of bamboo leaf ash (BLAsh) and silica
fume (SF). The pozzolanic activity is evaluated by using a conductometric method. In this method the electrical conductiv-
ity in a BLAsh/Ca(OH)2 and SF/Ca(OH)2 solution is measured with the reaction time. Latter, a kinetic-diffusive model is
applied which allows computing the kinetic parameters of the pozzolanic reaction. The values of these parameters, specifi-
cally the reaction rate constant, characterize the reacting process and allow evaluating quantitatively the pozzolanic activity
of these materials. The application of other experimental techniques employed in this research [X-ray diffraction (XRD) and
scanning electron microscopy (SEM)], support the results coming from the conductometric method. The results show that
BLAsh and SF are formed fundamentally by amorphous silica with a high pozzolanic activity. The comparison of BLAsh
with SF allows concluding that both have a similar reactivity with reaction rate constant of 4.78 × 10−1 and 5.11 × 10−1 h−1
respectively. This fact reveals the importance of this agricultural residue for their use in the manufacture of blended cements.

Keywords Materials characterization · Pozzolanic activity · Bamboo leaf ash · Kinetic parameters · Silica fume

Statement of Novelty of future eco-efficient cements, residue which could replace

silica fume.
The novelty of the paper is that for the first time a qualitative
and quantitative comparison of the pozzolanic behavior of
bamboo leaf ash and silica fume is made. For the first time, Introduction
the reaction rate constant for silica fume is reported, allow-
ing quantitative and rigorous comparison with bamboo leaf A worldwide practice is the use of waste materials that
ash. The authors think that the knowledge generated in this have pozzolanic properties in the production of mortars
work is novelty and will notably contribute to the possibility and concretes. The knowing and assessment of the pozzo-
of analyzing the use of bamboo leaf ash in the production lanic activity of supplementary cementitious materials is
very important for the production of base cement materials
* Ernesto Villar‑Cociña more ecofriendly, with minor cost and with technological
evillar@uclv.edu.cu advantages.
The concrete is the most used building material in the
1
Department of Physics, Central University of Las Villas, world, its annual production ascends to more than 10 billion
54830 Santa Clara, Cuba
tons produced in modern industry [1]. It has been estimated
2
University of Sao Paulo, P.O. Box 23, Pirassununga, that by 2050 its production will increase to approximately
SP 13635‑900, Brazil
18 billion tons annually [2]. However, these productions
3
Eduardo Torroja Institute (CSIC), c/Serrano Galvache, 4, have a negative effect on the environmental, due to ­CO2
28033 Madrid, Spain

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1628 Waste and Biomass Valorization (2020) 11:1627–1634

emissions caused during the cement Portland manufactur- bamboo cultivation and important quantities of bamboo
ing process. The cement industry alone is estimated to be are processed. This generates large volumes of solid waste.
responsible for about 7% of all the ­CO2 generated worldwide This waste is burned in open spaces, which contaminates
[3]. For this reason, the partial substitution of the cement by the environment. However, if these residues are calcined in
materials with pozzolanic properties in concrete production appropriate conditions and places, they can become in future
is a worldwide practice. eco-efficient pozzolans. Several works have recently been
One of the best and most popular pozzolans is the silica published in this area of research, with promising results
fume (SF). This pozzolan can be added to Portland cement that need to continue being studied and deepened [27–35].
in the range of 9–15% by mass of cement [4], although the The methods generally used to evaluate the pozzolanic
existing regulations limit it to 10% [5]. Several advantages activity of agricultural residues are really qualitative meth-
have the use of SF: increase pore refinement; improvement ods that focus on the qualitative aspect of the pozzolan-lime
of strength at early age, stiffness, better behavior against the (CH) reaction (by comparison the behaviors of a pozzolanic
alkali-aggregate reaction and improve the sulphate resist- material with another). These methods do not take into
ance [6]. account the quantitative aspect of the pozzolan-lime (CH)
Nevertheless, despite from the various advantages of SF, reaction (computing of kinetic parameters of the reaction).
there are also disadvantages such as: the increase in heating Villar-Cociña et al. [28] calculated the kinetic parameters
and in the heat of hydration developed in the SF blended (reaction rate constant and activation free energy) in BLAsh/
cement matrixes [7], and the very expensive cost, which is CH solution, by applying a diffusive-kinetic model devel-
significantly higher than that of OPC per ton. The limited oped by the same authors in previous works [14, 36–38].
amount available of SF and the very expensive cost (about This allowed characterizing quantitatively the pozzolanic
0.25–0.50 €/kg in Europe) [8] limits its application in the behavior between the CH and the Brazilian bamboo leaves
cement industry, especially in developing countries. These ashes. Frías et al. [29] conducted a scientific study of a
reasons give a high motivation for the search of other mate- Brazilian bamboo leaf ash (BLAsh) in order to analyze the
rials with similar functions that allow substituting the SF. behavior of this ash in mixed cements made with 10% and
As alternatives to the high cost and small amount of SF 20% by mass of BLAsh. The results showed that the bamboo
available are being valued agricultural wastes, which are ash is constituted by amorphous silica as the only main com-
generating serious environmental and social problems, ponent and possesses a high pozzolanic activity (reaction
by their accumulation in landfills and uncontrolled burn- rate constant of the order of ­10−1 h−1).
ing. Agricultural residues such as sugarcane bagasse ash, Recently, the qualitative and quantitative pozzolanic char-
sugar cane straw ash, rice husk ash, wheat straw ash, hazel acterization of a Cuban bamboo leaves ash was carried out,
nutshell ash etc, have been valued as pozzolanic materials the results showed a high pozzolanic reactivity (reaction
for using as cement replacement material [9–18]. The use rate constant around of 1.2 h−1). In this paper the influence
of these residues in construction will offer many benefits, of calcining temperature on the pozzolanic activity and the
taking into account that it represents a fundamental axis of kinetic parameters of the reaction was analyzed [38].
the strategy of the Circular Economy [19]. The use of these However, a comparative study on the pozzolanic activity
agricultural wastes in the cement industry as supplementary of SF and BLAsh in pozzolan/CH systems and a quantita-
cementitious materials (SCMs) will contribute to the more tive characterization taking into account the kinetic param-
environmentally friendly and economically effectiveness of eters of the pozzolanic reaction have not been localized in
this industry and the construction materials [20, 21]. the international literature. For this reason, one of the main
At present, one of the residues that have generated great objectives of this research was to explore and establish
interest as an active addition to cement is bamboo leaf ash, the preliminary scientific basis for the feasibility of using
which is obtained from the calcination of the leaves. It is BLAsh instead of SF (scarce and expensive even in devel-
known that bamboo can be used as a construction material oped countries) in mortars and concrete.
and is the natural resource that grows fastest and with the The present paper shows a comparison between bamboo
highest yield. In addition, a large number of bamboo crops residues calcined at 600 °C and SF. The electrical conductiv-
are available. On the other hand, the use of vegetable rein- ity of the pozzolan-CH solution is measured experimentally
forcement fibers in cementitious materials has shown very while the reaction takes place and is correlated with the con-
hopefulness results. In the case of bamboo, its fibers are centration of Ca(OH)2. The fit of the kinetic-diffusive model
excellent in this respect, have an ecofriendly nature that and by non-linear regression methods allows the calculation of
also provide a very economical and socially useful outlet the kinetic parameters of the pozzolanic reaction (reaction
[22–26]. However, not all bamboo waste is used as fibers; rate constant mainly) in the Blash/CH and SF/CH systems,
other waste is generated such as the bamboo leaf that is not which allows a rigorous quantitative evaluation of the poz-
used as fibres. In several countries, there are large areas of zolanic activity of these materials. Chemical compositions,

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Waste and Biomass Valorization (2020) 11:1627–1634 1629

X-ray diffraction patterns (XRD), scanning electron micros-

copy (SEM) and calculation of the kinetic parameters of the
pozzolanic reaction supported the study. The results show a
similar pozzolanic reactivity of BLAsh in comparison with
SF.

Materials and Methodology

Materials

The silica fume used in this study was supplied from Elkem
Co., Ltd. (Sao Paulo, Brazil). Elkem Microsilica has a
85–98% amorphous silicon dioxide ­(SiO2) in the form of
microscopic spherical particles. According to the supplier
company (Elkem Microsilica), the average diameter of these
particles is 0.1–0.15 µm.
In Fig. 1a, photograph of the silica fume used in this
investigation is shown.
The bamboo leaves were collected in the University of
São Paulo, Pirassununga Campus, Brazil.
Bamboo leaves were initially calcined at 400 °C for
60 min to remove organic matter in a muffle furnace (JUNG
10010, Brazil). Then, calcined at 600 °C for 60 min with a
heating rate of 10 °C/min´with this temperature the highest
pozzolanic reactivity of BLASh has been obtained, reported
by several authors [27, 28, 38]. Figure 1b shows the ash used
in the current study, which showed a gray color. The curves
of the particle size distribution of the ashes, determined
using a laser diffraction particle analyzer (CILAS, Brazil) in
liquid mode, showed that all ashes have a fine granulometry
with average or majority size of 21.41 µm.
Fig. 1  a Appearance of silica fume, b bamboo leaf ash
Both pozzolans (SF and BLAsh) were ground and sieved
below 45 µm.
The saturated calcium hydroxide solution used was pre- perspective of pozzolanicity. It is of great importance to
pared with deionized water and Ca(OH)2 with 95% mini- investigate how soon the pozzolanic material reacts with
mum purity. The solution was obtained by mixing and stir- CH and, once reaction takes place, the rate at which activity
ring the Ca (OH)2 in excess with deionized water for 20 min is occurring.
at 500 rpm. Subsequently, the solution was kept at rest for One hundred milliliters of saturated solution of Ca (OH)2
30 min and finally the solution was filtered. was used and mixed with 2.10 g of bamboo leaf ash (this is
the ratio used by other authors in this type of experiment)
Pozzolanic Activity Method and they were stirred magnetically. The conductivity meas-
urements are started at the moment of mixing the ash with
There are many experimental methodologies that allow a the CH solution. A Digimed microconductimeter (DM-32)
qualitative or quantitative determination of pozzolanic activ- was used at a temperature of 40 ± 1 °C permanently. A cali-
ity [39, 40]. In this work the electric conductivity method bration curve that allows correlating the concentration of CH
was used, which was used by some authors in other scien- with the conductivity of the CH solution was applied [31].
tific works [36, 37, 41–44]. This method allows following
the variation of the electrical conductivity of the calcium Characterization Techniques
hydroxide-pozzolan solution with the reaction time. The use
of methods based on the electrical conductivity of an aque- The ashes of bamboo leaves were chemically characterized
ous suspension of pozzolan/CH has significantly reduced by using X-ray fluorescence, with a PANalytical Axios XRF
the times needed to characterize these materials from the spectrometer.

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1630 Waste and Biomass Valorization (2020) 11:1627–1634

X ray diffraction was used for studying the mineral- Results and Discussion
ogical composition of ashes. The powder method was
employed by using an X-ray diffractometer, PANalytical, Chemical and Mineralogical Characterization
model X Pert PRO with X Celerator detector.
The Scanning Electron Microscopy was used for the The main elements (expressed as oxides) present in bamboo
morphological analysis and microanalysis of the samples. ash and silica fume are shown in Table 1. Silica ­(SiO2) is the
A Philips XL 30 microscope that also provides images of main oxide in both ashes. The content of amorphous ­SiO2 in
secondary electrons and backscattered electrons, together SF is significantly high, while it has small amounts of iron,
with an integrated EDAX system was used. magnesium, alumina, calcium and alkaline oxides. BLAsh
shows a lower amount of S ­ iO2 (80.4%) than SF (87.5%),
other oxides are present in smaller amounts.
Mathematical Model The loss of ignition (LOI) was determined by submitting
the ash for 2 h at 1020 °C and determining the weight loss
A kinetic-diffusive model was used in the pozzolan/CH of the ash.
system to determine the kinetic parameters of the pozzo- Figure 2 shows the XRD pattern for the BLAsh and SF
lanic reaction [36, 37]. It is known that these coefficients materials. For both materials, the shape of the band is simi-
represent a good quantitative criterion to evaluate the poz- lar. The XRD pattern of bamboo ash shows a broad band
zolanic activity of the materials. The model is: located around 2θ = 15°–30°, which corresponds to its
( ) ( ( )) highly amorphous nature. In the bamboo ash (Fig. 2a) the
C − Ct 0.23 × exp − 3t𝜏 × −1 + exp 𝜏t × 1
𝜏 presence of crystalline minerals was not detected; while SF
𝜉= o =1− (Fig. 2b) is almost completely amorphous, it contains some
Co Co De rs2
( ) crystalline phases such as: quartz, halite and magnetite, in
0.23 × exp − 𝜏t × 1
addition to the vitreous phase.
(1)
𝜏
+ − Ccorr
Co krs2
Pozzolanic Activity of Bamboo Ash: Comparison
where ­De is the effective diffusion coefficient; K is the reac- with Silica Fume (SF)
tion rate constant; C­ o is the initial conductivity of the solu-
tion; 𝜏 is a constant of time (for this time the radius of the With the aim of comparing the pozzolanic activity of bam-
nucleus of pozzolan decreases to 37% of its average initial boo ash with SF, the conductometric method was employed
radius ­rs). for both samples. The results of the pozzolanic activity for
Ccorr is a correction term, which represents the CH con- the BLAsh calcined at 600 °C and SF samples are shown in
centration remainder that is not consumed in the reaction. Fig. 3. The variations of the conductivity with the reaction
(Co − Ct)/Co represents the relative loss of conductivity times (h) for the pozzolan/calcium hydroxide (CH) suspen-
(dimensionless magnitude). sion are presented in this figure.
Ct is the absolute loss of conductivity with time for the The electrical conductivity of the pozzolan/CH systems
pozzolan/CH solution. diminish significantly, which is only attributed to the poz-
The pozzolanic reaction is a chemical reaction that zolanic reaction between amorphous silica and CH to give
develops in stages, which may have usually very different C–S–H gels. This produces the corresponding decrease of
resistances. It is known that the stages with the highest the CH concentration in the solution. At early ages of the
resistance, that is, the slowest, control the process. There- pozzolanic reaction, a considerable variation (loss) of con-
fore, there may be different behaviors in correspondence ductivity is obtained for both BLAsh and SF samples. For
with the controlling stage: diffusive control [described by long periods of time the stabilization of the curve is reached.
the 2nd term of Eq. (1)], kinetic control (3rd term) and For this time the reaction has practically finished.
mixed kinetic-diffusive control (both terms). More details According with the above-mentioned result, it might be
on the elaboration and considerations of the model can be possible to conclude that a greater reactivity is qualitatively
found in Refs. [36, 45]. observed for BLAsh, followed by SF. However, another

Table 1  Chemical composition Material Chemical composition [oxides (%)]

of the BLAsh and SF
SiO2 Al2O3 Fe2O3 MgO CaO Na2O K2O SO3 Cl P2O5 LOI

BLAsh 80.4 1.22 0.71 0.99 5.06 0.08 1.33 1.07 0.18 0.20 8.04
SF 87.5 0.51 2.13 2.81 0.45 2.55 2.15 0.79 0.45 < 0.001 0.62

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Waste and Biomass Valorization (2020) 11:1627–1634 1631

(a) 600 important factor that must be taken into account when an
evaluation of the reactivity is carried out is the difference
500 Bamboo ash between the initial and final conductivities (stabilized elec-
trical conductivity) in the different solutions pozzolan/CH
400 (a major difference, the reactivity of the material will be
higher) [46]. This could be related with the amount con-
counts

300 sumed of calcium hydroxide, a great difference corresponds

to a greater consume of CH in comparison with a minor
200 difference.
For the case of the materials shown in Fig. 3, is evident
100
that SF consumes more CH than the BLAsh. However, a
high reactivity of BLAsh is appreciated from the qualita-
0
10 20 30 40 50 tive point of view comparable to SF, a highly expensive
2θ (°) pozzolan.
It is clear that qualitatively, it is very difficult to have an
(b)
16000 Q: Quartz SiO2
accurate idea of the pozzolanic activity. For that reason an
Q
Ha: Halite NaCl
Silica fume
evaluation from the point of view quantitative of the pozzo-
Ma: Magnetite
Fe3O4 lanic reactivity that involves all this aspects and that allows
12000 the computation of the kinetic parameters is very important.
Ha
After the conductivity test (50 h of reaction), the SEM
counts

observation was carried out. Figure 4 shows the formation of

8000
Ma C–S–H gels for BLAsh and SF samples, rough areas having
Q a foil-like morphology [47, 48].
4000
Quantitative Analysis of the Pozzolanic Activity:
Determination of the Kinetic Parameters
0
10 20 30 40 50
2θ (°) The kinetic–diffusive model (Eq. (1)) was fitted for all sam-
ples. Figure 5a, b show the relative loss of conductivity
Fig. 2  XRD pattern of the bamboo for a Bamboo leaf ash, b Silica plotted against reaction time for the BLAsh/CH and SF/CH
Fume systems. The continue line is the curve of the fitted model.
The model in its variants of kinetic, diffusive and mixed
control (kinetic-diffusive) was successively fitted to the rela-
tive loss of conductivity-time data.
A rigorous evaluation of the fitting process of the model
10
to the experimental data was carried out. Several important
statistical parameters were analyzed in detail, such as the
correlation coefficient r, the multiple determination coef-
8
Silica Fume ficient ­(R2), the sum of residual squares (RSS), 95% confi-
dence intervals, residuals dispersion, residuals probability
Conductivity (mS/cm)

6 Bamboo leaf ash and analysis of variance. This allowed us to conclude that,
in the case of SF sample; a kinetic–diffusive control regime
predominated showing the best correspondence with the
4 experimental data. Therefore, both processes determine the
general speed of the whole process. For the case of BLAsh,
2
a kinetic control predominated, which means that the rate of
chemical interaction on the surface of the nucleus of the poz-
zolan particle is slower than the rate of diffusion of the reac-
0
0 10 20 30 40 50
tant through the layer of reaction product that forms around
Time (h) the nucleus. This result could be related to a high porosity
of the reaction product layer in this material, which causes
Fig. 3  Variation of conductivity with reaction time for BLAsh cal- a rapid diffusion process. Further explanations of the model
cined at 600 °C and SF characteristics can be found in the Refs. [36, 45].

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1632 Waste and Biomass Valorization (2020) 11:1627–1634

(a) 1.0

0.8

0.6
r=0.9918

(Co-Ct)/Co
R2= 0.9942
0.4

0.2

0.0

0 10 20 30 40 50
Time (h)

(b) 1.0

0.8

0.6
(Co-Ct)/Co
r=0.9906
0.4 R2=0.9934

0.2

0.0
0 10 20 30 40 50
Fig. 4  SEM micrographs after the reaction (50 h of reaction) with Time (h)
calcium hydroxide showing the CSH gels for: a BLAsh calcined at
600 °C; b SF
Fig. 5  Relative loss of conductivity plotted against reaction time for:
a BLAsh calcined at 600 °C, b silica fume. Filled circle—experimen-
tal, Line—model
Table 2 shows the values of the parameters (𝜏 , D and K).
The correlation and multiple determination coefficients r and
­R2 are shown in Fig. 5a, b. silica fume, which is considered one of the best worldwide
Taking into account the values of the kinetic parameters pozzolans.
it is possible to conclude that both BLAsh and SF have a
very high and similar reactivity. The silica fume has a reac-
tivity slightly higher (larger K, but of the same order) than Conclusions
the BLAsh calcined at 600 °C.These results agree with the
qualitative analysis described in the section above entitled In accordance with the results reported in this research, the
“Pozzolanic activity of bamboo ash. Comparison with silica following conclusions arise:
fume (SF)”.
The pozzolanic reactivity for SF and BLAsh calcined at (a) The main oxide present in BLAsh and SF ashes is S ­ iO2
600 °C is two orders of magnitude greater in the value of with a percentage of 80.4 and 87.4% respectively, fol-
the reaction rate constant than the reactivity of sugar cane lowed by CaO (5.06%), A ­ l2O3 (1.22%) for Blash and
straw ash (SCSA) and rice husk ash (RHA) and three orders MgO (2.81%) and F ­ e2O3 (2.13%) for SF. Other oxides
greater than bagasse ash from sugar cane (SCBA), which are present in both samples in smaller amount. Each
are considered highly pozzolanic residues in the technical material contains silica in adequate quantities to qualify
literature [36, 37]. them as pozzolanic material.
This result allows us to state that the ashes of bamboo (b) According to XRD analysis, the pattern of bamboo
leaves are an excellent pozzolanic material comparable to ash shows a broad band located around 2θ = 15°–30°

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Waste and Biomass Valorization (2020) 11:1627–1634 1633

Table 2  Reaction rate constants, parameter, ­Ccorr parameter and statistical parameters for BLAsh calcined at 600 °C and SF

Material (ash) 𝜏 (h) Reaction rate constant ­(h−1) Ccorr Correlation Coefficient of multiple Residual
coefficient (r) determination ­(R2) sum of
squares

BLAsh 4.3 ± 0.05 (4.78 ± 0.09). ­10−1 0.22 ± 0.002 0.9918 0.9942 0.022
SF 4.1 ± 0.1 (5.11 ± 0.08). ­10−1 0.17 ± 0.003 0.9906 0.9934 0.068

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313782/2013-0, Project PVE), CNPq (ref: 306386/2013-5). FAPESP 14. Villar-Cociña, E., Frías, M., Morales, E.V.: Sugar cane wastes as
(Process No. 2018/10719-6) for its financial support and the Collabora- pozzolanic materials: application of mathematical model. ACI
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