Construction and Building Materials 96 (2015) 65–75

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Construction and Building Materials

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

Laboratory processing of Colombian rice husk for obtaining amorphous

silica as concrete supplementary cementing material
Dimelsa Salazar-Carreño a, Rafael Guillermo García-Cáceres b,⇑, Oscar Orlando Ortiz-Rodríguez c
a
Pontificia Universidad Javeriana, Bogota, Colombia
b
Uniagustiniana, Avenida Ciudad de Cali No. 11B-95, Bogota, Colombia
c
Universidad de Pamplona, Pamplona, Colombia

h i g h l i g h t s

 Is evaluated the physical and chemical analyses of Colombian’s RHA.

 A laboratory research methodology is presented for obtain concrete mixtures.
 The best result obtained was: AT, type II (650 °C), GT (240 min) and CRP 40%.

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

Article history: Rice husk is an agro-industrial waste with few applications. However, its elevated amorphous silica con-
Received 6 August 2014 tent has turned it into a promising raw material, especially due to its possibility to be transformed into a
Received in revised form 16 March 2015 cement supplement for concrete mixtures. Investigating plant materials as new sources of high quality
Accepted 26 July 2015
amorphous silica has a number of important advantages resulting in a process that may involve fewer
Available online 6 August 2015
steps than usual. Determining the suitability of the specific silica materials obtained from Colombian rice
husk ash for them to be used in concrete mixtures involves the assessment of several features such as
Keywords:
percentage of amorphous silica, particle size, surface area and specific gravity. The current work focused
Rice husk ash
Amorphous silica
on the laboratory ash production process, whose appropriate temperature, grinding and burning time
Cement supplement conditions were assessed through their effect on the compressive strength of concrete cylinders
Sustainable industry supplemented with the obtained materials. This, in turn, ensures obtaining an elevated percentage of
23 factorial design amorphous silica and provides an adequate conceptual framework for industrial production.
Ó 2015 Elsevier Ltd. All rights reserved.

1. Introduction
Rice husk being an agro-industrial waste with few applications,
its current abundance has turned it into an environmental prob-
lem. This makes it necessary to find profitable and environmentally
friendly uses for this material [3]. On the other hand, the search for
new sources of high quality amorphous silica is currently a signif-
icant scientific and technological endeavor [11]. Amorphous silica
prepared from plant raw materials has a number of important
advantages over that obtained from minerals. In evaluating two
grinding methods in terms of the physical and chemical character-
istics of the obtained rice husk ash (RHA), Martinez et al. [12] made
⇑ Corresponding author. Tel.: +57 (1) 4193200.
E-mail addresses: dimelsa.salazar@javeriana.edu.co (D. Salazar-Carreño), rafael.
garcia@uniagustiniana.edu.co (R.G. García-Cáceres), oscarortiz@unipamplona.edu.
co (O.O. Ortiz-Rodríguez).
two interesting findings: the possibility to carry out the whole pro-
cess in fewer steps than usual and, due to the stable chemical com-
position of plants, a final product containing only a narrow range of
metal oxide impurities.
The use of RHA as a cement supplement for concrete mixtures
depends critically on determining its production and usage condi-
tions. In producing electricity from rice husk incineration, the
resulting ash has been used as a partial substitute for clinker in
cement ([4,15]). The application of modern technologies to this
type of process has yielded ashes of such good quality that they
are assimilated to silica fume, a well-known, highly valued product
employed in the preparation of high performance concrete
([13,16]). This study explores optimum production of supplemen-
tary cementing materials from Colombian rice husk, particularly
focusing on the effects produced on concrete compressive strength
(CS) at two setting times by the factors rice husk burning time and
temperature, ash grinding time, and percentage of cement

http://dx.doi.org/10.1016/j.conbuildmat.2015.07.178
0950-0618/Ó 2015 Elsevier Ltd. All rights reserved.
66 D. Salazar-Carreño et al. / Construction and Building Materials 96 (2015) 65–75
replacement with the obtained materials. The work determines the
characteristics of local rice husk and the obtained RHA, which it
compares to materials reported in previous studies. The experi-
mental parameters were particularly adopted following the sug-
gestions provided in the literature and the available technological
conditions.
Thus, the present paper was aimed at determining adequate
laboratory conditions for the stable and sustainable production of
amorphous silica through the combustion of Colombian rice husk,
which is produced in large amounts and, therefore, at low costs.
This is one of the most relevant problems involved in the sustain-
able development of the rice and cement industries, which gener-
ate considerable environmental impacts due to their strong
national presence. Hence, the current work expects to contribute
to the modernization of these industries by promoting efficiency,
productivity and sustainability.
2. Background
The use of rice husk amorphous silica as a cement supplement
has been under investigation for several decades. Hence, the cur-
rent section reviews some of the most relevant works found in
the literature on the topic. Ortiz-Rodríguez and Castells [18] pre-
sent a review on sustainability, based on LCA, in the construction
industry. Van Tuan [26] studied the use of RHA as an additive for
high performance concrete. In that experiment, rice husk was sub-
jected to uncontrolled burning at temperatures reaching no more
than 780 °C. The obtained ashes were ground in a vibrating ball
mill for 45 min, with the aim of reducing particle size and improv-
ing surface area. The experimental results allowed concluding that
when average particle size was less than 7.3 lm, the obtained RHA
material had about the same pozzolanic activity as silica fume. This
parameter increases as particle size decreases, but it does not
change significantly beyond 5.6 lm. Therefore, the material in
question was found to be adequate for concrete mixtures.
The work of Zain et al. [28] describes the production of RHA as a
cement supplement in concrete mixtures. The ashes were obtained
through a continuous combustion process initially supplied with
air, after which they were allowed to cool down and finally ground.
During the first two hours, the average temperature of the oven
was 500–600 °C; then it was reduced as the burning process went
on. Fluorescence and X-ray diffraction analyses allowed determin-
ing the amorphous nature of the obtained silica material and its
SiO2 content (87%), which, in turn, revealed the good quality of
the obtained RHA.
Ganesan et al. [7] evaluated optimal percentages of cement
replacement with RHA by focusing on the strength and permeabil-
ity of the resulting concrete materials. They burned a RHA residue
in an industrial furnace where the temperature was increased at a
rate of 200 °C per hour until it reached the desired threshold of
650 °C. This process took 3 h and 15 min, after which combustion
was allowed to proceed under controlled conditions for an addi-
tional hour. Then, the system was cooled down. The material was
pulverized to a mean grain size of 3.8 lm before it was used as a
substitute for cement. This investigation concluded that it is possi-
ble to replace 30% (weight) of ordinary Portland cement with RHA
without any adverse effect on the strength and permeability of
concrete.
Nehdi et al. [15] evaluated the performance of Egyptian RHA as
a concrete additive using a new Torbed-reactor-based burning
technology. Three combustion tests were carried out at 750 °C,
830 °C, and 750 °C, the latter additionally receiving air injection
from the outside. The performance of the RHA material thus
obtained was compared to that of an American (U.S.A) prime qual-
ity one produced in fluidized bed. The tested material demanded
less grinding time (GT) than the reference one, without substan-
tially increasing the demand for water and superplasticizer, which
is an advantage over silica fume. As a function of the amount of
added RHA, the CS of concrete was improved up to a maximum
of 40% in 56 days, which overcomes the performance of silica fume.
This study demonstrated that the technology in question is eco-
nomical and can be used in rice-producing countries, not only to
develop a very effective supplementary cementing material, but
also to reduce the environmental impact of this rice byproduct’s
uncontrolled burning.
Safiuddin et al. [20] used finely powdered gray RHA obtained by
a conventional heat treatment. This material, featured by its hon-
eycomb microstructure, exhibited larger surface area
(2326 m2/kg) and smaller particle size (412 m2/kg) values than
those of cement, together with an accelerated pozzolanic activity
index of 122.4% and a 93.6% silica content. After mixing different
RHA/cement proportions to prepare hardened concrete mixtures,
the properties of the obtained materials were observed to improve
as a function of increased RHA content. The micro-filling and poz-
zolanic effects of this cement supplement were found to improve
the structure and microstructure of the concrete’s pores.
Excellent hardness properties were obtained with 15% RHA.
Salas et al. [21] analyzed RHA samples with and without chem-
ical pre-treatment then subjected to thermal treatment. The sam-
ples were analyzed for color, amorphous silica content, particle
size distribution and surface area. A controlled burning process
was conducted in a programmable furnace heated at a rate of
10 °C/min until reaching 600 °C, a temperature that was main-
tained for three hours in both experiments. In order to improve
the performance of these pozzolanic materials, they were pulver-
ized in a ceramic ball mill for 90 min. The cement substitution tests
resulted in two concrete mixtures (the 5% and 10% chemical treat-
ment intensity ones) of increased water demand and CS, the latter
overcoming the records of 100% Portland cement. In this way, the
newly obtained supplement exhibited a similar behavior to that of
silica fume.
Martínez et al. [12] analyzed RHA production in a bubbling,
atmospheric, fluidized bed reactor operating at 750 °C under
excess air levels of 40%, 82.5% and 125% and a fluidization speed
of 0.14 nm/s in all cases. They found that air excess correlated
inversely with reaction temperatures, which, in turn, held a direct
correlation with rice husk thermochemical transformation effi-
ciency and silica content in RHA. The process showed good poten-
tial for producing ashes with high contents of amorphous silica
(>93%) and low carbon levels (3.5%), which can therefore be used
as pozzolanic materials in the construction industry.
Della et al. [6] obtained RHA from the raw material produced by
a local industry in Brazil. In an electric furnace they conducted a
series of heating cycles at a rate of 10 °C/min. The samples were
kept at temperatures of 400, 500, 600 or 700 °C for 1, 3 or 6 h
and then ground (10, 40 or 80 min cycles) to reduce the size of
ash particles and increase their specific surface area. The 6-h treat-
ment at 700 °C produced the highest silica content and was there-
fore selected for grinding (80 min), which rendered particles
smaller than 33 lm with a specific surface area increase that went
from 54 to 81 m2/g. A 95% purity silica powder was obtained
through this calcination treatment. Despite the thermal treat-
ments, the silica materials thus obtained remained in an amor-
phous state. The authors concluded that RHA is an alternative
source of silica with elevated surface area.
Xu et al. [27] obtained ashes by treating rice husk in an electric
furnace heated at a rate of 20 °C/min. Several samples were kept at
temperatures of 500, 600, 700 or 800 °C for 2 h. Then they were
ground in a vertical ball mill for 2 h. The obtained RHA material
was assessed for specific surface area (77.42 m2/g), average particle
size (150 nm), and SiO2 content (91.74%). These parameters
 D. Salazar-Carreño et al. / Construction and Building Materials 96 (2015) 65–75 67

exceeded those of ordinary silica fume (20–28 m2/g, 0.1–0.3 lm Although the best results are obtained closely below 750 °C, the burning tem-
perature should not exceed this threshold. When this is the case, crystalline silica
and 75–96%, respectively), thus showing the strong reactive poten-
is formed, which prevents the interaction between RHA and cement particles.
tial of RHA as a pozzolan. Table 1 summarizes the chemical and
physical properties of the different materials obtained by the above
mentioned authors. 3.1.2. Gravimetric analysis
According to the literature, particle size in this type of experiment is usually
equal to or less than 17 lm, partly because the samples are usually ground after
3. Materials and methods
the heat treatment. In order to determine particle size, a gravimetric analysis was
conducted, which involved putting the RHA material through a sieving system of
The literature review allowed identifying the methods and evaluating the char-
downward decreasing mesh diameters: 8 (2.36 mm), 30 (600 lm), 50 (300 lm),
acteristics employed by researchers to determine ash sample suitability for replac-
100 (150 lm), 170 (90 lm), 200 (75 lm), 325 (45 lm). Subsequently, the material
ing cement in concrete mixtures. On these grounds, the rice husk material was
falls on a receiver that should ideally keep at least 90% of the screened material,
incinerated in a furnace to obtain the ashes. Subsequently, the samples that exhib-
thus indicating that the average particle size is less than 45 lm. The importance
ited similar features to those described in the literature were chosen for concrete
of this process has to do with the way particle size influences ash pozzolanic activ-
cylinder experimentation, which was carried out under a 23 factorial design with
ity [26].
different cement replacement percentages (CRPs), in order to evaluate CS after 3,
Five hundred grams of RHA were weighted and put through the sieve assembly
7 and 28 days, as shown in Fig. 1. This is the most frequently used experimental
(orderly arranged from coarse to fine mesh size numbers), which was then agitated
design for studies involving the behavior of concrete mixtures as affected by varia-
in a sieve shaker for 15 min for the material to sift through the system. Next, the ash
tions in their determining factors and their interactions [9,17,22].
fraction retained on each screen was weighed to determine the corresponding
percentage. The results are presented in Table 4.
3.1. Preparation of rice husk ash The gravimetric analysis sought to determine the heat treatment that allowed
obtaining the highest percentage of material meeting the desired particle size.
The rice husk material used for the experiments was obtained from the com- Table 4 shows that the highest percentage of material retained at the bottom sieve
pany Molinos Roa Espinal, located in the Department of Tolima (Colombia). In terms (97.93% < 45 lm) corresponded to the 650 °C treatment, while the smallest
of its physical properties, this material exhibits some similarities with the one used percentage (less than 90%) was obtained at 750 °C.
by Martínez et al. [12], basically regarding the residual and ash percentages. The
results of the physical and chemical analyses of the raw materials are shown in
Table 2.
3.1.3. Mineralogical analysis
Raw rice husk was subjected to the heat treatments in a furnace at tempera-
Subsequent to the gravimetric analysis, the mineralogical analysis allowed
tures of 600, 650, 700 or 750 °C for a 3-h burning period. The selection of the tem-
determining the percentage of crystalline and amorphous material present in the
peratures and the combustion time was based on previous research by Xu et al.
ash samples. This was done by assessing the presence of cristobalite and tridymite,
[27], Della et al. [6] and Salas et al. [21], who used similar burning equipment.
which should ideally be found in low percentages. The results of this analysis are
The shes they obtained were assessed not only for particle size, but for the percent-
summarized in Table 5.
ages of unburned material and amorphous silica as well. Particle size was assessed
As seen in Table 5, the 650 °C and 120-min-burning-time treatment allowed
through the ash fractions resulting from the sieving process.
obtaining the best results in terms of the percentage of unburned material and
the percentage of the sample deposited at the bottom of the sieving system. The
3.1.1. Percentage of unburned material assessment current results are consistent with those reported by Xu et al. [27], Della et al. [6]
This process sought to remove volatile constituents, transform fixed carbon into and Salas et al. [21], who proceeded under similar operating conditions, except
gaseous components such as CO2, and determine the final percentage of carbon in for the fact that some of them applied chemical or drying treatments before
the ash sample. This evaluation allows ruling out unfavorable quality samples. burning.
A 300 g sample of compact rice husk material was weighed on a stainless steel
pan scales for general laboratory purposes. Then, in order to eliminate volatile com-
pounds, the sample was burned in a furnace at a temperature of 500 °C. 3.2. Evaluation of the RHA-amended concrete mixture
Subsequently, the temperature was increased and maintained according to the dif-
ferent treatments, the results of which allowed calculating the corresponding per- CS is concrete’s most common performance parameter. In this work, it was
centages of unburned materials as defined in Eq. (1) (Table 3). assessed in concrete cylinders amended with the ash materials produced in the lab-
  oratory, on days 3, 7 and 28 after they were prepared. The literature shows that the
W incinerated material
% of unburned materials ¼ 100   100 ð1Þ CS of concrete depends on raw material quality and proportion in the mixture [14].
W sample
There is a significant variety of methods to investigate the effects of different

Table 1
Comparison of RHA physical and chemical properties as reported by various researchers.

Features References
Van Tuan Zain et al. Ganesan et al. Nehdi et al. Safiuddin et al. Salas et al. Martínez et al. Della et al. Xu et al.
[26] [28] [7] [15] [20] [21] [12] [6] [27]
Chemical properties
SiO2 (wt%) 87.96 86.49 87.32 94.6 93.6 99.00 93.3 94.95 91.71
Al2O3 (wt%) 0.3 0.01 0.22 0.3 – <0.01 0.15 0.39 0.36
Fe2O3 (wt%) 0.52 0.91 0.28 0.3 – 0.13 0.14 0.26 0.9
CaO (wt%) 1.14 0.50 0.48 0.4 – 0.49 0.38 0.54 0.86
Na2O (wt%) – 0.05 1.02 0.2 – <0.32 0.01 0.25 0.12
K2O (wt%) 3.29 2.70 3.14 1.3 – 0.06 2.2 0.94 1.67
SO3 (wt%) 0.47 – – – – – 0.24 – –
MgO (wt%) – 0.13 – 0.3 – <0.07 – 0.90 0.31
TiO2 (wt%) – 0.00 – 0.03 – 0.02 – 0.02 –
P2O5 (wt%) – 0.69 – 0.3 – 0.11 0.64 0.74 –
MnO (wt%) – 0.07 – – – 0.02 0.18 0.16 –
C (wt%) – 3.21 – 1.0 – – – – –
Ignition losses 8.55 8.45 2.10 1.8 – – 2.6 0.85 3.13
Physical properties
Average particle size 7.3 – 3.80 7.15 6 17 – – –
(lm)
Specific gravity (g/cm3) 2.1 – 2.06 2.05 – 2.08 – – –
Specific surface area 19.2 – 36.47 – 2.32 274 – – 77.42
(m2/g [%])

(–): unavailable data. wt%: weight%.

68 D. Salazar-Carreño et al. / Construction and Building Materials 96 (2015) 65–75

Fig. 1. Research methodology.

Table 2 Table 3
Chemical composition and physical characteristics of raw rice husk. Percentages of unburned material according to temperatures and burning times.

Characteristic Value Temperature Burning time % of unburned material

Apparent density (g/cm3) 0.100 600 120 3.22
Residual moisture (wt%) 8.9 650 120 2.07
Ashes (wt%) 13.71 700 120 1.26
Superior calorific power (Cal/g) 3.910 750 120 0.58
Percent composition (weight)
Source: Original data by the authors.
SiO2 13.21
Al2O3 0.078
Fe2O3 0.027
CaO 0.098
3.2.1. Experimental design and factors affecting quality
MgO 0.07
A 23 full factorial design was used to assess the effects that the studied factors
SO3 0.002
and their interactions had on the response variables. These factors and their differ-
K2O 0.24
ent levels are described below:
Na2O 0.009

Source: Prepared by the authors from data by ‘‘Alienergy’’.
variables on the quality of concrete, namely the Taguchi [19,23], response surface
[2,25] and factorial design [5,24] techniques; the latter being the one applied in
the current study to evaluate the effects of the main factors and their interactions.
U Ash Type: The temperatures of the thermal treatments differentiate the RHA
materials thus obtained. The current analysis was applied to the materials trea-
ted at 600 °C and 650 °C, which were respectively named type I-600 and type
II-650. This choice was based on their exhibiting the best particle sizes and per-
centages of unburned material and amorphous silica (mineralogical analysis).
 D. Salazar-Carreño et al. / Construction and Building Materials 96 (2015) 65–75 69

Table 4 Table 6
RHA gravimetric analysis results. Factors and factor levels.

Treatment temperature (°C) Percentage of material at the Factors Levels

bottom of the sieving system (%)
AT Type I-600 °C Type II-650 °C
600 96.55 GT 30 min 240 min
650 97.93 CRP 20% 40%
700 93.16
750 89.24 Source: Experimental data by the authors.

Source: Experimental data commissioned by the authors to ‘‘Centrek’’ Technological Table 7

Center. Analysis of variance for compressive strength at 7 days (coded units).

Source DF SS. SM adj. F P value

U Grinding time: Subsequent to the burning treatments and the corresponding AT 1 59,511 59,511 8713.71 0.000
analyses, the obtained ashes were ground for 30 min to achieve smaller particle GT 1 5944 5944 870.34 0.000
sizes, for them to approach those of cement. Four additional grinding periods of CRP 1 5032 5032 736.72 0.000
1 h each (summing up to a total of 240 min) allowed reaching a AT  GT 1 37,328 37,328 5465.57 0.000
less-than-15-lm particle size (micromilled RHA). AT  CRP 1 0.1 0.1 0.01 0.093
U Cement replacement percentage: Following standard NTC 31 (Norma Técnica GT  CRP 1 2382 2382 348.78 0.000
Colombiana 31 – Colombian Technical Norm 31) [10], the mixtures prepared AT  GT  CRP 1 4757 4757 696.58 0.000
to make the concrete cylinders were amended with RHA replacing cement by Error 16 109 6.8
20% and 40%. The selection of these percentages was complemented with the Total 23 115,063
works of Safiuddin et al. [20], Ganesan [7] and Salas (2010). [10] specifies that
the pozzolan content of a concrete mixture must range between 15% and 50% of DF: Degrees of Freedom; SS.: Square Sum; SM adj.: Square Mean (adjusted).
its total mass. The water/cement ratio (0.48) and the proportions of the other Source: MinitabÒ 16.2.3.
components of the mixture were kept constant in all trials. Table 6 summarizes
the factors affecting concrete quality and their experimental levels.
Table 8
Pareto analysis of compressive strength.
According to the provisions of [1], the CS of pozzolanic cements must be at least
11 MPa (112.7 kgf/cm2) at 7 days and 21 MPa (214.14 kgf/cm2) at 28 days. Although Evaluated Conclusions
the parameter is not specified for 1 and 3 days, it should ideally be greater than the variable
standard.
CS at 7 days The most significant factor was found to be AT, and the
(kgf/cm2) most significant interaction the one between AT and GT.
3.2.2. Conduction of the experiment The only non-significant effect was the AT  CRP
Using the micromilled and ordinarily ground ash materials resulting from the interaction
treatments listed in Table 6 and 80/20% and 60/40% cement/RHA mixture cylinders CS at 28 days All factors and their interactions were found to be
were prepared, keeping a constant water/cement ratio of 0.48. (kgf/cm2) significant
The factorial design used for the experiment was run on a MinitabÒ 16.2.3 and
17.1.0 commercial software package. Each experiment was repeated thrice, for a Data prepared by the authors.
total of 24 measurements per response variable.

4. Results and discussion Table 9

Analysis of variance for compressive strength at 28 days (coded units).
A statistical analysis was conducted to determine the best Source DF SC sec. MC adjusted. F P value
experimental condition and the influence of the factors under
AT 1 104,769 104,769 20315.46 0.000
assessment. For such purpose, concrete CS measurements at 3, 7 GT 1 27,983 27,983 5426.03 0.000
and 28 days were checked for normality, variance homogeneity CRP 1 14,519 14,519 2815.34 0.000
and independence of residues, respectively using the Kolmogorov AT  GT 1 1512 1512 293.21 0.000
Smirnov, Levene, and Durbin-Watson tests [8]. The assumptions AT  CRP 1 22,946 22,946 4449.48 0.000
GT  CRP 1 20,668 20,668 4007.74 0.000
of these models were satisfied by the CS data obtained at 7 and
AT  GT  CRP 1 1481 1481 287.08 0.000
28 days, but the 3-day data did not meet the residue independence Error 16 83 5
assumption, which led not to apply the factorial analysis to this Total 23 193,960
variable. The 7 and 28 day data were subjected to the statistical
DF: Degrees of Freedom; SS.: Square Sum; SM adj.: Square Mean (adjusted).
analysis in order to determine the best results and their Source: MinitabÒ 16.2.3.
corresponding factor levels.

4.1. Determination of significant responses to the studied factors analyses, the AT  GT interaction was found not to be significant.
The CRP correlated inversely with CS at 7 days (see Table 8).
Table 7 presents the effects of factor level changes on the The same statistical procedure was carried out for CS at 28 days.
average response variable (CS at 7 days). As concluded in previous The results are shown in Table 9.
At a confidence level of 95%, the null hypotheses for effects A, B,
C and interactions AT  GT, AT  CRP, GT  CRP and AT  GT  CRP
Table 5
were rejected, thus implying that they significantly affect the
X-ray diffraction mineralogical analysis.
response variable.
Treatment Amorphous Cristobalite% Quartz% Hematite%
temperature (°C) material%
600 70 20 10 N/P
4.2. Interpretation of active effects
650 75 15 10 N/P
700 50 27 23 N/P Main Effect and Interaction Effect graphs were used for the
750 N/P 45 44 10 analysis of active effects, which is intended to identify those condi-
N/P = not present. tions of the process that allow optimizing the response variables.
Source: Experimental data commissioned by the authors to ‘‘Alienergy’’. The results are summarized in Table 10 and detailed in Appendix A.
70 D. Salazar-Carreño et al. / Construction and Building Materials 96 (2015) 65–75

Table 10
Effects of the main factors and their interactions.

Variables Analysis of the effects Cube graph results

CS at 7 days The significant Interaction Effects (GT  AT and GT  CRP) were analyzed. When the GT of The best CS result was obtained by combining type II
type II ash (650 °C) was prolonged, CS was also markedly increased. The opposite result (650 °C) micromilled ashes, GT (240 min) and a 40% CRP
was obtained with type I ash (600 °C). When the CRP was 20%, CS did not change
significantly regardless of GT (30 or 240 [micromilled] min). Yet, this parameter changed
considerably when the CRP was shifted to 40% and micromilled ashes (240 min) were
used
CS at 28 days Provided that in this case all interactions were found to be significant, they were all
analyzed. As to the AT  GT interaction, CS increased with the use of both types of
micromilled ashes. However, type II ash rendered better results than type I ash. Regarding
the AT  CRP interaction, when the GT was 240% CS was also markedly increased. When
using type I ash, positive changes in the CRP determined CS decrements. With regards to
the GT  CRP interaction, CS was increased by positive changes in both factors. To
conclude, the best CS record at 28 days was obtained by using micromilled type II ash at a
40% CRP

Table 11
Best operation conditions for the maximization of concrete compressive strength. Finally, at 7 and 28 days, the 100% concrete (standard) cylinder
showed lesser CS values than those of the one prepared with ashes
Variable Condition Prediction
from the best experimental conditions.
2
CS at 7 days (kgf/cm ) Type II ash 520.90
GT: 240 min
CRP: 40% 5. Conclusions
CS at 28 days (kgf/cm2) Type II ash 755.06
GT: 240 min
CRP: 40% The rice husk material used for the present research bears cer-
tain similarity with those employed by other researchers who have
Source: The authors.
worked in Colombia with local materials, mainly regarding resid-
ual and ash percentages.
According to the CS tests applied to the concrete cylinders pre-
pared in the experiment, burning temperature proved to be more
Table 12
Comparison between the best experimental concrete mixture and a control cylinder
influential than burning time, which is consistent with the results
(100% cement). of previous research works in which time was kept constant.
The optimal treatment temperature ranged from 600 °C to
Characteristic Standard (100% cement) Best sample (80%:20%)
700 °C. Burning time was found to correlate negatively with the
CS (kgf/cm2) at 7 days 400 520.90 percentage of unburned material, but neither the percentage of
CS (kgf/cm2) at 28 days 543 755.06
retained material, which is directly related to particle size, nor
N/A: not applicable. the percentage of amorphous material were significantly affected.
Experimental data prepared by the authors. However, the cooling rate was observed to be an important
(though hard to control) laboratory factor affecting ash production
through elevated percentages of amorphous silica.
Table 11 shows the predicted values of the studied variables, The different temperature treatments (600, 650, 700 and
which were calculated using an adjusted regression model (Eqs. 750 °C) allowed obtaining RHA materials with similar physical
(2) and (3)) whose coefficients and equations were obtained with and chemical characteristics to those reported in previous works.
the aid of a Minitab software package. The 650 °C treatment rendered the best results regarding particle
size and composition. These features are of great importance since
Y 1 ¼ 40; 641 þ 4980X 1 þ 1574X 2  1448X 3 þ 1944X 4 they affect the chemical reactions with cement leading to the for-
þ 996X 6 þ 1408X 7 ð2Þ mation of hydration products.
To conclude, CS values of 520.90 and 755.06 kgf/cm2 can be
obtained at 7 and 28 days, respectively, by replacing 40% of cement
Y 2 ¼ 63; 497 þ 6607X 1 þ 3415X 2  2460X 3  794X 4 with micromilled RHA material treated at 650 °C. These CS values
þ 3094X 5 þ 2935X 6  785X 7 ð3Þ are consistent with the minimum standards set by [1] for poz-
zolanic cements. However, it is important to take into account that
where CS varies over time. We suggest further studying the relationship
between the three analyzed factors, since elevated GT and CRP val-
Y1: CS at 7 days (kgf/cm2) ues did not render consistent CS results with either AT.
Y2: CS at 28 days (kgf/cm2) Comparing the CS results of the reference concrete cylinder
X1: AT (100% Portland cement) to those of the current experiment’s best
X2: GT RHA-cement mixture (650 °C, 240 min, 40%), the latter was
X3: CRP observed to exceed the former by 30.22% and 39.05% at 7 and
X4: AT * GT 28 days, respectively.
X5: GT * CRP
X6: AT * CRP
X7: AT * GT * CRP Adenda

The CS results were compared to those of a cylinder made of The promotion of sustainable building principles in developed
100% cement without ash incorporation (Table 12): and developing countries is closely associated to progress in new
 D. Salazar-Carreño et al. / Construction and Building Materials 96 (2015) 65–75 71

materials with lower environmental impact along their lifecycle. In Appendix A

this sense, RHA constitutes an innovative ecological alternative, as
far as it resorts to a renewable raw material source and improves A.1. Determination of significant factor effects on the response
concrete properties. variables

Acknowledgments A standardized Pareto chart was employed to determine the fac-

We express our gratitude to Centrek Technology Center and
Alienergy for providing physical and financial resources for the
development of the laboratory and additional tests required for
this work.
tor effects (AT, GT and CRP) and their interactions on the response
variables (CS at 7 and 28 days). These results were confirmed later
on through analysis of variance (ANOVA) at a 95% confidence level.
Fig. A1 shows the Pareto chart corresponding to CS at 7 days, while
Table 7 shows the corresponding ANOVA of each factor.

Source: Minitab® 17.1.0

Fig. A1. Standardized Pareto chart for compressive strength at 7 days.

Source: Minitab® 17.1.0

Fig. A2. Pareto standardized diagram for compressive strength at 28 days.

72 D. Salazar-Carreño et al. / Construction and Building Materials 96 (2015) 65–75

Table A1 Fig. A1 shows that the most significant factors are AT and its
Effects of the main factors and their interactions. interaction with GT. The only non-significant effect was AT  CRP.
Factors Effects These results are confirmed by the 7-day-CS ANOVA at a 95% con-
AT 99.59 fidence level.
GT 31.47 The ANOVA presented in Table 7 shows that the p value is lower
CRP 28.96 than the level of significance (a = 0.05) for all factors and interac-
AT  GT 78.88 tions, exception made of GT  CRP. In consequence, the null
AT  CRP 0.09
GT  CRP 19.93
hypothesis is rejected for factors A, B and C, and for interactions
AT  GT  CRP 28.16 AT  CRP, GT  CRP and AT  GT  CRP, thus confirming the conclu-
sion obtained from the standardized Pareto chart.
Source: MinitabÒ 16.2.3.

Source: Minitab® 17.1.0

Fig. A3. Compressive strength Main Effects at 7 days.

Source: Minitab® 17.1.0

Fig. A4. Interaction Effects of the studied factors on compressive strength at 7 days.
 D. Salazar-Carreño et al. / Construction and Building Materials 96 (2015) 65–75 73

Source: Minitab® 17.1.0

Fig. A5. Cube diagram for compressive strength at 7 days.

Source: Minitab® 17.1.0

Fig. A6. Main Effects for compressive strength at 28 days.

A.1.1. Compressive strength at 28 days
Fig. A2 confirms the ANOVA results (95% confidence level)
shown in Table 9.
All the factors and their interactions were found to have a
significant effect on CS at 28 days, their p values were all lower
than the level of significance (a = 0.05).
A.2. Interpretation of active effects
The analysis of active effects resorted to Main Effect and
Interaction Effect diagrams, which allow identifying the processing
conditions under which CS can be maximized. The results are
summarized in Table A1.
Table A1 illustrates the average behavior of the response vari-
able in face of changes in the level of the studied factors. As also
concluded in previous analyses, the AT  CRP interaction was
observed not to be significant, which is made evident by its corre-
sponding low effect value, when compared to those of the other fac-
tors. In the case of CRP, a negative effect value was observed,
implying that changes in this factor bring about a CS decrement
at 7 days. These results are consistent with those of Figs. A3 and A4.
The Main Effect diagrams (Fig. A3) for CS at 7 days showed bet-
ter results when the concrete cylinders were made of micromilled
type II ash at a 20% CRP.
In this case, the only analyzed interactions were AT  GT and
GT  CRP (Fig. A4), because AT  CRP was not significant. As to
74 D. Salazar-Carreño et al. / Construction and Building Materials 96 (2015) 65–75

Source: Minitab® 17.1.0

Fig. A7. Compressive strength at 28 days as affected by the interaction between the studied factors.

Table A2 AT  GT, increments in the latter when using type II ash deter-
Effects of the main studied factors and their interactions for R-28.
mined remarkable CS increases, whereas considerably lower incre-
Factors Effects ments were observed with the use of type I ash. Regarding
AT 132 GT  CRP, when the CRP was 20%, CS did not change significantly,
GT 68.29 regardless of GT. Yet, this parameter changed considerably when
CRP 49.19 the CRP was 40% and GT was raised to 240 min. Thus, articulating
AT  GT 15.88
interactions AT  GT and GT  CRP, and looking forward to increas-
AT  CRP 61.84
GT  CRP 58.69 ing CS at 7 days, it is advisable to use type II (650 °C) micromilled
AT  GT  CRP 15.71 ash, GT (240 min) and a 40% CRP. This conclusion is confirmed by
the cube diagram shown in Fig. A5.
Source: MinitabÒ 16.2.3.

Fig. A8. Cube diagram for compressive strength at 28 days.

 D. Salazar-Carreño et al. / Construction and Building Materials 96 (2015) 65–75
A.2.1. Compressive strength at 28 days
Also at 28 days, increasing the CRP reduced CS. This observation
is confirmed by the magnitudes of interactions AT  GT and
AT  GT  CRP, which are not as significant as those of the Main
Effects or the other Interaction Effects. Figs. A6 and A7 illustrate
the graphic analysis of these effects (see Table A2).
The main factor analysis (Fig. A6) indicates the use of type II ash,
a GT of 240 min and a CRP of 20%.
Fig. A7 shows CS at 28 days as affected by the studied interac-
tions, all of which were found to be significant. AT  GT shows that
CS increased when using a 240 min GT, whereas a further increase
was obtained by using type II ash. As to AT  CRP, an increment in
the latter factor when using type II ash was the only combination
that increased CS. GT  CRP showed a similar performance to AB. In
effect, using a GT of 240 min, CS increased with either 20% or 40%
CRP. In turn, changes in CRP brought about similar results to
AT  CRP. Hence, it can be concluded that the adequate conditions
to prepare the concrete mixture and obtain better CS results at
28 days are similar to those found at 7 days. This conclusion is
confirmed by the cube diagram shown in Fig. A8.
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