Leon Et Al. 2020 - Areia de Osório + CCA + CC PDF

Journal of Testing and Evaluation
doi:10.1520/JTE20180763 / Vol. 48 / No. 3 / 2020 / available online at www.astm.org
Helena Batista Leon,1 Mariana da Silva Carretta,1 Maurício Birkan Azevedo,1

Matteo Conti,2 and Nilo Cesar Consoli3
Statistical Analysis of the Influence of

Curing Time and Temperature on
Compressive Strength of Sandy Soil
Stabilized with Sustainable Binder
Reference
H. B. Leon, M. da Silva Carretta, M. B. Azevedo, M. Conti, and N. C. Consoli, “Statistical Analysis
of the Influence of Curing Time and Temperature on Compressive Strength of Sandy Soil
Stabilized with Sustainable Binder,” Journal of Testing and Evaluation 48, no. 3 (May/June
2020): 2441–2458. https://doi.org/10.1520/JTE20180763
ABSTRACT
Manuscript received October 22, Rice husk ash (RHA) is a by-product of the incineration of rice husk, a process whose objective
2018; accepted for publication is the generation of thermal and electrical energy. Carbide lime (CL) is a residue of acetylene
November 5, 2019; published
online December 26, 2019. Issue
gas production. Agricultural-industrial wastes, like RHA and CL, have great potential applica-
published May 1, 2020. tions in earthworks, mainly in the regions where these residues are produced. This research
1
evaluates the potential use of RHA mixed with CL as a binder used to improve strength proper-
Department of Civil Engineering,
Universidade Federal do Rio ties of sandy soils, substituting portland cement. Different curing temperatures (23°C and
Grande do Sul, 99 Osvaldo Aranha 40°C) and curing periods (7 and 28 days) of the compacted sandy soil-RHA-CL blends were
Ave., Porto Alegre, Rio Grande do evaluated to determine the importance of such changes on the strength of the blends. Studies
Sul 90040-060, Brazil
have been carried out to quantify the unconfined compressive strength (qu) as a function of a
2
Department of Civil and novel index called porosity/binder. The aim of this index is to measure the influence of porosity
Environmental Engineering,
and binder content on blends’ properties, considering the combination of the amounts of RHA
Politecnico di Milano, 32 Leonardo
da Vinci Sq., Milano 20133, Italy and CL as the binder. The results show that higher values of qu are obtained with the reduction
of porosity and with the increase of binder content. Curing temperature acts as a catalyzer and
3
Department of Civil Engineering,
accelerates pozzolanic reactions between RHA and CL. For the purpose of verifying the effect
Universidade Federal do Rio
Grande do Sul, 99 Osvaldo Aranha of the investigated controllable factors—γd, RHA, CL, and curing type—in the response variable
Ave., Porto Alegre, Rio Grande do qu, an analysis of variance was performed. Based on that, it was possible to verify that the types
Sul 90040-060, Brazil
of curing during 28 days at 23°C and for 7 days at 40°C are statistically equivalent. It increases
(Corresponding author), e-mail:
consoli@ufrgs.br, https://orcid. the possibility of choice for engineering design because these results mean that the engineer
org/0000-0002-6408-451X may choose an appropriate curing period and temperature in accordance with project require-
ments and average temperatures in the site construction.
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by ASTM reserved); Wed
International, Aug Harbor
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2442 LEON ET AL. ON STATISTICAL ANALYSIS OF SOIL-BINDER
Keywords
soil stabilization, sustainability, curing time, curing temperature, strength
Introduction
In situ soils do not always meet design requirements and may need improvement in order to be transformed into
appropriate earthwork materials. This is often accomplished by physical or chemical stabilization of the prob-
lematic soils. Chemical stabilization usually employs portland cement; however, the development of alternatives,
such as reusing agricultural-industrial wastes, often results in environmental and economic benefits. Sandy soils
do not react with lime, but the addition of ashes to these mixtures enables the occurrence of pozzolanic reactions
between the calcium hydroxide (Ca(OH)2) of the lime and the silica (SiO2) from the added ash, improving
strength, stiffness, and endurance properties.1–3
This research evaluates the use of rice husk ash (RHA) and carbide lime (CL) as a binder, enhancing geo-
technical properties of soils (a sandy soil is tested in this study). The use of these materials aims to reduce wastes,
acting as an environmentally sustainable binder for geotechnical applications, especially in the regions where
these residues are generated. Ideal locations include anywhere that is near industrial plants that produce acetylene
gas or agricultural regions where rice is cultivated, where the cost of material transportation is greatly lessened by
the fact that it is produced close by.
The RHA is an agricultural-industrial residue with great potential to be used as a pozzolanic addition and
partial replacement of portland cement in soil-cement dosages because of the high concentration of SiO2 accu-
mulated by the rice plant. The incineration of rice husk has been used as a way to reduce its volume and generate
thermal and electrical energy. However, burning still produces another waste, the RHA. According to Juliano,4 the
rice husk produces approximately 20 % of its weight in ash when incinerated. Yet, as stated by Ali, Adnan, and
Choy,5 every 4 tons of rice generates 1 ton of husk.
In Brazil, approximately 12 million tons of rice were harvested in 2017.6 Based on the presented data, it can
be estimated that approximately 3 million tons of husk were generated as residue, and that about 600,000 tons of
ash could have been produced from the incineration of all the husk coming from that harvest.
Studies of Behak7 stabilized a Uruguayan sand soil with RHA. The author evaluated the California bearing
ratio, the stress-strain behavior on triaxial tests, unconfined compressive strength (qu) and split tensile strength,
and durability under wetting and drying cycles. The stabilization proved to be efficient, allowing the use of these
materials in pavement subbase layers.
CL is a residue from acetylene gas production. The world production of acetylene gas was approximately
500,000 tons in 2014, whereas the CL production as a waste was approximately 1,423,000 tons.8 Thailand
produces 21,500 tons/year of CL, whereas China produces approximately 100,000 tons/year.9 According to
Saldanha et al.,10 Brazil currently produces 6,000 tons/year of acetylene gas and generates approximately
17,100 tons/year of CL.
Amorphous SiO2 (and alumina [Al2O3]) reactivity in an alkaline environment (e.g., Ca(OH)2, sodium
hydroxide) produces pozzolanic reactions. Such reactions might result in stable products, such as calcium silicate
hydrate (and calcium aluminate hydrate), with required binding assets.11 As mentioned by Massazza,12 the poz-
zolanic chemical reaction between SiO2 and Al2O3 of coal fly ash, hydrated lime [Ca(OH)2], and water (H2O)
shapes CSH (calcium silicate hydrated) and CAH (calcium aluminate hydrated).
The pozzolanic reactions of fly ash-CL blends are slow at ambient temperatures of 23°C and, therefore, demand
long curing times to achieve some target values of strength.11 Higher temperatures (40°C and 60°C) accelerate the gain
of strength of fly ash-CL blends investigated by Saldanha and Consoli,11 in comparison to standard laboratory curing
temperature (23°C), showing that temperature acts as a catalyzer. The studies of Rao and Asha13 on sand-lime-fly ash
specimens showed that larger strength values are developed at higher curing temperatures, even in a shorter period.
The strength of specimens cured in a steam water bath at 80°C for 24 h developed strength values twice as large as those
of specimens cured at room temperatures of 25°C for 28 days.
Copyright by ASTM Int'l (all rights reserved); Wed Aug 5 11:22:58

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of Testing and Evaluation
LEON ET AL. ON STATISTICAL ANALYSIS OF SOIL-BINDER 2443
Studies of Jaturapitakkul and Roongreung14 proposed a new cementitious material composed of a mix-
ture of calcium carbide residue (CCR) and RHA that has the potential to be used in concrete works that do
not require high compressive strength. The authors studied the mechanical behavior of mortars with differ-
ent amounts of CCR and RHA and found that mixtures with the proportions of 50 % of each material gave
the highest compressive strength, which reached 15.6 MPa after 28 days of curing and increased to 19.1 MPa
after 180 days. Those results suggest that the UCS of the specimens was about 2 times lower than the control
mortar made of portland cement, but the new cementitious material had the advantage of not containing
portland cement; additionally, the strength of mortar is the result of the pozzolanic reaction of the two ma-
terials. The authors suggest that other studies should perform durability tests in order to prove the efficacy of
this new binder.
Because pozzolanic reactions are affected by many factors (such as porosity, amounts of RHA and CL, curing
temperature, and curing period), a dosage methodology is needed to assess mechanical behavior of these blends.
Thus, this study supports its analysis with the use of the porosity/volumetric binder content (η/Biv) index, which
considers the volumetric binder content as the sum of volumetric RHA content and volumetric CL content of
sandy soil-RHA-CL blends. A statistical analysis of variance (ANOVA) demonstrates the significance of the said
controllable factors on the strength of the specimens.
Experimental Program
MATERIALS
Osorio sand was originally from the region of Osorio, Southern Brazil. It can be classified, according to Unified
Soil Classification System (USCS), as SP.15 The soil is a nonplastic uniform fine sand, with rounded particle
shape and unit weight of the grains of 26.3 kN/m3. According to the classification for highway purposes,16
Osorio sand can be classified as A-3. The grain size distribution (fig. 1) shows a mean effective diameter
(D50) of 0.16 mm.
The RHA was obtained from a rice company from the region of Alegrete, also in Southern Brazil. The
company incinerates the rice husk in a process involving controlled temperatures to generate thermal and electric
energy, producing RHA as a by-product. The unit weight of the grains is 22.0 kN/m3, and the grain size
distribution (fig. 1) shows that the D50 value is 0.022 mm. The main constituent of rice rusk ash is amorphous
SiO2 as shown in Table 1. Also, the mineralogical characterization (fig. 2) revealed the presence of cristobalite,
which is a polymorph of SiO2 that forms at high temperatures.
The CL utilized throughout this investigation is the residue collected from an acetylene gas production plant
located in Sapucaia do Sul, Southern Brazil. CL has a unit weight of solids of 21.9 kN/m3, and the grain size
FIG. 1
Grain size distribution
of Osorio sand, RHA,
and CL.

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TABLE 1
Chemical characterization
Chemical RHA CL
SiO2 93.6 3.10

Al2SO3 0.26 0.46
CaO 1.20 74.0
Fe2O3 0.20 0.26
K2O 2.91 ND
TiO2 ND ND
SO3 0.40 0.54
MgO ND 0.72
MnO 0.50 ND
P2O5 0.85 ND
Na2O ND ND
Others 0.10 …
Note: ND = not detected.
FIG. 2
X-ray diffraction analysis
of rice husk ash.
distribution (fig. 1) shows the D50 value of 0.02 mm. Calcium oxide (CaO) is the main constituent of the CL used as
the alkaline activator (Table 1). The mineralogical characterization indicates the presence of the minerals portlandite
[Ca(OH)2], calcite (CaCO3), which was formed because of the carbonation process, and graphite (C) (fig. 3).
Distilled water was employed for all specimens molded, whereas tap water was used for submersion of the
specimens before unconfined compression tests, in order to minimize suction.
METHODS
The minimum amount of lime required to enable reaction with the pozzolanic material and the sandy soil was
achieved by the initial consumption of lime method (ICL) initially proposed by Eades and Grim,17 adapted by
Rogers, Glendinning, and Gerber,18 and standardized by ASTM International.19 A saturated solution of lime in

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FIG. 3
X-ray diffraction analysis
of carbide lime.
distilled water has a pH value of 12.40 at 25°C. This pH is required to maintain the reaction between lime and any
reactive components in the material to be stabilized.13
The ICL method defines the amount of lime required to achieve and maintain a pH of 12.4. Thus, following
the procedure required by ASTM D6276-99a(2006), Standard Test Method for Using pH to Estimate the Soil-Lime
Proportion Requirement for Soil Stabilization,19 it was determined that the lowest percentage of lime in the blend
should be at least 2 %. Therefore, increasing lime contents (5, 8, and 11 %) were tested.
Proctor compaction tests (using standard effort) were carried out in order to assess optimum moisture con-
tent and maximum dry unit weight (γd) of Osorio sand, RHA, and CL mixtures. The contents of RHA, based on
sandy soil dry masses, were 10, 20, and 30 %, and the content of CL was 8 % (by the sum of amounts of sandy soil
and RHA) for all blends used for these tests. Figure 4 presents the results of the three standard Proctor tests
carried out in this research.
Molding and Curing of Specimens

The molding points for specimens submitted to strength (unconfined compression) tests carried out had a target
moisture content of 14 % (approximately optimum moisture content obtained from the Proctor Compaction
test). They also had three different γd values (14.5, 15.5, and 16.5 kN/m3). These three values of γd were chosen
based on the Proctor compaction tests (16.5 kN/m3 is approximately the maximum value of γd that could be
molded considering the three amounts of RHA). CL contents chosen were 5, 8, and 11 % considering
international experience with soil-lime blends.20 RHA contents chosen were 10, 20, and 30 % by the dry mass
of sandy soil. The total number of specimens molded for strength tests was 81, and the variations of RHA and CL
contents and curing temperatures are shown in Table 2.
A target γd for a given specimen was then established through the sum of dry masses of the sandy
soil-RHA-CL blend divided by the total volume of the specimen. According to equation (1), as proposed
by Consoli, Dalla Rosa, and Saldanha,21 porosity (η) is a function of γd of the blend, contents of sandy
soil (S), RHA and CL, and unit weights of solids of sandy soil (γss), rice husk ash (γsRHA), and carbide lime
(γsCL).

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FIG. 4 Proctor compaction tests for sandy soil, RHA, and CL mixtures.
TABLE 2
Specifications of the specimens molded for strength tests
Dry Unit Weight, kN/m3 RHA Content, % CL Content, % Curing Type, Days-°C
14.5 10, 20, 30 5, 8, 11 7-23; 7-40; 28-23

15.5 10, 20, 30 5, 8, 11 7-23; 7-40; 28-23
16.5 10, 20, 30 5, 8, 11 7-23; 7-40; 28-23
8" #" #9
< γd S RHA CL =
η = 100-100 100
+ 100
+ 100
(1)
: 100
S
+ RHA
100 + 100
CL γsS γsRHA γsCL ;
To represent the influence of the content of RHA and CL in a single index, the volumetric binder content
(Biv) is adopted. The index represents the influence of the sum of contents of these materials on blends’ properties.
Equation (2) shows the calculation of the latter index, which is based on the volumetric contents of RHA (VRHA)
and CL (VCL) by the total specimen volume (V).
mRHA mCL
V RHA +V CL γsRHA + γsCL
Biv = = (2)
V V
Through the combination of porosity and volumetric binder content, it is possible to quantify the influence
of both materials in a single value, considering the RHA+CL to be an innovative cementitious material made of a
pozzolanic material (RHA) and an activator (CL). As stated in the equation (3), it is possible to evaluate the qu of
the treated soil as a function of the η/Biv, being A, D, and E scalars.22
−E
η
qu = A (3)
ðBiv ÞD
The molding procedure for the tests’ specimens was carried out as follows: soil, RHA, CL, and water were
weighted; subsequently, the solid materials were blended until a uniform consistency was attained. At this point,

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water was added and mixed together until a uniform consistency was obtained again. Specimens were then stati-
cally compacted in three layers, inside a cylindrical split mold, according to the method proposed by Ladd,23 so
that each layer reached the specified γd. The top of each layer had to be slightly scarified, except for the upper one.
Specimens were then cured either in a moist room at 23°C ± 2°C and relative moisture of approximately 95 % or
in a steam room at 40°C ± 2°C with the same relative moisture. The moist room generally follows ASTM C511-13,
Standard Specification for Mixing Rooms, Moist Cabinets, Moist Rooms, and Water Storage Tanks Used in the
Testing of Hydraulic Cements and Concretes.24
The cylindrical specimen measurements are 50 mm in diameter and 100 mm in height. After molding pro-
cedures, all specimens were measured (diameter and height) with a precision of 0.01 mm and weighted with an
accuracy of 0.01 g. Appropriate specimens should obey the following tolerances: γd: degree of compaction between
99 and 101 % of the target value; measurement: diameter within ± 0.5 mm and height within ± 1 mm; moisture
content: within ± 0.5 %. In order to minimize suction, 24 h before carrying out testing (6 or 27 days after mold-
ing), specimens were submerged in a water tank.21,22
Unconfined Compression Tests

Unconfined compression tests have been carried out in many experimental programs in order to assess the ef-
fectiveness of soil stabilization with cement, lime, and binders. Tests carried out in this research followed the
requirements of ASTM D5102-09, Standard Test Method for Unconfined Compressive Strength of Compacted
Soil-Lime Mixtures,25 and had a displacement rate of 1.14 mm/min to determine qu of blends. Figure 5A–C
shows a specimen before, during, and after the unconfined compression tests, respectively.
In order to attain a more complete analysis and optimize the laboratory process, only one specimen for each
combination was created. Because of this optimization, it was possible to expand the ranges of γd values and
amounts of lime and RHA analyzed with a limited number of specimens.
The total number of specimens molded for strength tests was 81 with 3 variations of RHA content, 3 var-
iations of CL content, 3 different curing conditions, and 3 different γd values.
Statistical Analysis
For an effective statistical analysis of the soil improvement previously discussed, it is necessary to define and
characterize the response variable and the parameters involved in the process. The response variable (qu) is
of the type larger-is-better because the goal is to maximize its measurable value.
Table 3 presents all the parameters participating in the process, including both the controllable factors and
the factors kept constant throughout the research. Coded levels were used for the curing type because it is a
qualitative variable, with levels −1, 0 and +1 corresponding to 7 days of curing at 23°C, 7 days at 40°C and
28 days at 23°C, respectively.
Based on the soil improvement international experience, the factors of greater relevance were selected to be
studied.3,11,20–22 Therefore, the ranges of controllable factors shown in Table 4 were investigated. The parameters
FIG. 5
Unconfined compressive
strength: (A) specimens
molded, (B) specimen
during the unconfined
compression test, and
(C) specimen after the
test.

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TABLE 3
Parameters in the statistical analysis
Parameter Range
3
Dry unit weight, kN/m 14.5 16.5
RHA content, % 10 30
Lime content, % 5 11
Curing type −1 +1
Moisture content, % 14
Soil type Osorio sand
Lime type Carbide lime
TABLE 4
Controllable factors
Independent Variable Number of Levels Real Levels

3
Dry unit weight, kN/m 3 14.5 15.5 16.5
RHA content, % 3 10.0 20.0 30.0
Lime content, % 3 5.0 8.0 11.0
Curing type 3 −1 (7 days − 23°C), 0 (7 days − 40°C), +1 (28 days − 23°C)
that are not investigated in this research have a fixed level, thus becoming constant throughout the process. These
are the moisture content and the types of soil and lime. The factors not controlled in the process, also called noise
factors, are responsible for the experimental error. Examples of these include the operator and the precision of the
measuring equipment.
From a statistical point of view, the randomness of experimental errors caused by noncontrollable factors
(noise factors) must be taken into account. These factors can be minimized by repeating the experiment, which
would involve molding more than one specimen of the same dosage. Because no repetitions were performed, an
existing statistical resource is the use of interactions that are usually not significant (ABC, ABD, ACD, BCD, and
ABCD) to estimate the error variance term.26
A complete crossover design with repetitions requires a large number of tests to be performed. Thus, the
number of tests increases rapidly as the number of factors increases. However, it is usually the main factors (A, B,
C, and D) and the first order interactions (AB, AC, AD, BC, BD, and CD) that are of interest to the analyst because
the remaining degrees of freedom correspond to higher order interactions (three, four, and more factors) and as
such are difficult to physically interpret.27
According to Box, Hunter, and Hunter,28 it is reasonable to assume that higher order interactions are not
significant, which means it is possible to obtain information about the main effects and low-order interactions
from a single execution of the experiment. Generally, this does not imply a significant loss of information, especially
when the number of factors increases.27 This type of experimental design is more feasible in practice because it
reduces the costs and the time of execution of the experiment because of the smaller number of tests demanded.
ANOVA
Considering that the research aims to analyze the influence of the curing type (temperature and period of time), as
well as the impact of the other controllable variables presented in Table 3 on the strength of the specimens, an
ANOVA was performed. It determines which of the controllable factors exert influence on the response variable
qu. The experimental project consists of a cross analysis of four controllable factors studied at three levels each, as
previously presented in Table 4.
The ANOVA was performed at a significance level of 95 %, which indicates that controllable factors with p
values of less than 0.05 are statistically significant. Assuming that the interactions between three and four

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factors were not significant and considering the lack of repetitions, these factors were used to estimate the mean
squared error.
Based on the ANOVA, a multiple comparison of means method was implemented to identify the independent
variables that have standard deviations that are different from each other. In this way, an optimal adjustment can be
established, adopting the levels of each controllable factor that provide efficiency and economy for the stabilized soil.
Results
UNCONFINED COMPRESSIVE STRENGTH RESULTS
Figure 6A–C shows the variation of qu for compacted Osorio sand-RHA-CL blends cured for 7 days at 23°C (A),
for 7 days at 40°C (B), and for 28 days at 23°C (C). It can be observed that strength is gained when the inde-
pendent variables γd, RHA content, and CL content are incremented, the latter being the least expressive graphi-
cally. Additionally, the different curing conditions showed influence on the strength gain of the specimens. The
increase in curing temperature (40°C) compared to curing at room temperature (23°C) resulted in an increase in
the strength values of the specimens, and the same was observed in the specimens cured during 28 days.
According to the Brazilian standard,29 which regulates the application of soil-cement in pavement base
layers, a minimum strength of 2.1 MPa is required after 7 days of curing. Although using alternative and recycled
materials (CL and RHA), it can be seen that the sustainable binder developed proved to be favorable for this
application. For the curing time of 7 days at room temperature (23°C) (fig. 6A), the most compact specimens with
higher pozzolan content, regardless of the amount of lime, obey the criterion. In the accelerated cure specimens
(7 days at 40°C) (fig. 6B), only those with γd values of 14.5 and 15.5, and amounts of 10 and 20 % of RHA,
regardless of the lime content, did not reach the minimum limit. Finally, virtually all specimens cured for 28 days
at 23°C (fig. 6C) reached and exceeded the limit of at least 2.1 MPa. The exception was two specimens with the
lowest compaction and RHA content, for the amounts of 5 and 8 % of lime. All of this information is compiled in
Table 5, in which the resistances of all test specimens tested are presented.
Studies of Ingles and Metcalf 3 present a prediction of qu for different types of soils stabilized with portland
cement contents varying between 0 and 10 %. For uniform sand, the authors suggest an average strength of 1 MPa
with the use of 5 % cement and approximately 4 MPa for additions of 10 % cement. Yet, Consoli, Cruz, and
Floss30 present a massive amount of data of qu of an artificially cemented uniform sand. The authors used Osorio
sand; different amounts of PC III: 1, 3, 5, 7, and 9 %; and curing periods of 2, 7, and 28 days. The authors obtained
the maximum strength of 1 MPa at 2 days, 2 MPa at 7 days, and 2.5 MPa at 28 days, for the specimens with the
highest cement content (9 %).
INFLUENCE OF THE η/Biv0.28

Figure 7 shows the variation of qu with η/Biv
0.28
. Diambra et al.31 used a mixture-modeling framework and the prin-
ciples of the critical state soil mechanics to denote the qu of soils treated with portland cement (considered as the
binder). These authors’ studies resulted in a theoretical model that shows a direct relationship between soil and port-
land cement properties and empirical scalars presented on equation (3), so a physical meaning to the data results is
attained. They showed the theoretical development that results in the following equation, in which K and a are scalars.
−a
η
qu = K 1 (4)
ðBiv Þa
The model suggests that the value of K is affected by the strength of cementitious bonds and the soil matrix;
however, the influence of the cementing agent is much more effective. The external exponent is considered to be
controlled by the properties of the soil matrix and related to the relation between the peak resistance and the soil
density. Based on previous experimental data, 1/a can be considered to be 0.28; therefore, the theoretical value is
3.57 (coming close to 3.60 used in this work).

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FIG. 6 Variation of (A) qu with the controllable factors for 7 days at 23°C, (B) qu with the controllable factors for 7 days at
40°C, and (C) qu with the controllable factors for 28 days at 23°C.
The use of the referred index allows estimating the behavior of all the different molding and curing char-
acteristics (3 different γd, RHA contents, CL contents, and types of cure) in just three curves and equations.
Equations (5)–(7) determine the behavior of qu for specimens cured for 7 days at 23°C, 7 days at 40°C, and
28 days at 23°C, respectively.

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TABLE 5
Experimental matrix
Unconfined Compressive Strength, MPa
γd, kN/m3
14.5 15.5 16.5
RHA, % RHA, % RHA, %
10 20 30 10 20 30 10 20 30
CL, % CL, % CL, % CL, % CL, % CL, % CL, % CL, % CL, %
Curing Type 5 8 11 5 8 11 5 8 11 5 8 11 5 8 11 5 8 11 5 8 11 5 8 11 5 8 11
−1 (23°C − 7 days) 0.2 0.2 0.3 0.5 0.5 0.7 1.0 1.2 1.0 0.3 0.3 0.3 1.0 0.9 0.9 1.4 1.7 1.5 0.4 0.4 0.4 1.2 1.3 1.2 2.2 2.1 2.3
0 (40°C − 7 days) 1.0 1.1 1.4 2.3 3.2 2.8 3.8 4.6 4.3 2.0 1.6 1.9 4.6 3.7 3.7 4.8 7.0 5.8 2.6 2.7 2.7 4.9 4.8 5.4 8.5 7.2 6.1
1 (23°C − 28 days) 2.0 2.0 2.2 3.2 3.1 3.4 4.3 4.3 4.1 2.3 2.5 2.7 4.8 4.3 4.1 5.5 5.6 6.7 2.7 3.0 2.8 5.4 4.8 4.8 7.0 6.9 5.9
FIG. 7 Variation of qu with η/Biv index for compacted Osorio sand-RHA-CL blends.
qu ðMPaÞ = 3.05 × 104 ðη=Biv 0.28 Þ−3.60 ½R2 = 0.78 (5)
qu ðMPaÞ = 1.19 × 105 ðη=Biv 0.28 Þ−3.60 ½R2 = 0.80 (6)
qu ðMPaÞ = 1.17 × 105 ðη=Biv 0.28 Þ−3.60 ½R2 = 0.65 (7)
Reasonable correlations (coefficient of determination [R2] = 0.78 – see equation (5), R2 = 0.80 – see equa-
tion (6), and R2 = 0.65 – see equation (7)) suggest that the models have the predictive ability to estimate values of
qu based on η/Biv0.28. The R2 was obtained by the least squares fit method.

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Once the power functions are the same for the three different equations, the scalars represent the strength
difference between the three curing types performed. It is observed that qu values are substantially lower for the
specimens cured at room temperature for 7 days, whereas the other two curing types do not show meaningful
difference between one another.
Furthermore, lower values of porosity (η) and higher values of volumetric binder content (Biv) result in
higher values of qu. This statement is also in accordance with the data presented by figure 6A–C, as an increment
in the compaction effort (increasing the γd) and in the amount of fines in the blends (increasing the contents of
RHA and CL) reduces the void ratio, and consequently, the porosity of the specimens. The increment in the
contents of RHA and CL also provides higher content of cementitious material.
As mentioned previously, the lowest strength value (qu) for soil-cement mixtures is 2.1 MPa, after 7 days of
curing, to be suitable to be employed as pavement base layer according to a Brazilian standard.29 By analyzing
figure 7 and equations (4) and (5), a target value of η/Biv
0.28
of 14.33 for specimens cured for 7 days at 23°C meets
this requirement, whereas when the curing temperature is increased to 40°C (considering only 7 days of curing),
the target value of η/Biv0.28 is 20.91. Therefore, higher values of porosity and lower values of volumetric binder
content can obey the standard requirements when the curing temperature increases, reducing costs because of the
decrease in compaction effort or in materials content.
It should be noted that the higher the value of η/Biv, the higher the porosity of the specimen (lower compaction
effort required) and the lower the cement content. It represents an economy in the amount of cement required for
soil stabilization and in the energy expended with compaction. When the curing temperature is increased, the costs
related to compaction and cementitious material are further reduced. It is also important to note that a single value
of Biv can be calculated by different amounts of pozzolanic material (in this case RHA) or lime (in this case CL),
which may be a decision depending on the materials availability near to the construction site.
In order to demonstrate that the RHA + CL binder could be a potential substitute of portland cement, some
specimens of a mixture of Osorio sand with RHA and type III portland cement (PC III) were molded. The
specimens were cast in a triplicate system and the mean of 3 specimens is shown in figure 7. It was chosen
to perform 3 points, varying the amount of RHA in the blend, being γd = 16.5 kN/m3, RHA = 10 %,
PCIII = 11 %; γd = 16.5 kN/m3, RHA= 20 %, PCIII = 11 %; and γd = 16.5 kN/m3, RHA= 30 %, PCIII = 11 %.
As it can be observed, the points fit the established curves of the specimens cured for 28 days at a temperature
of 23°C and for 7 days at 40°C. Also, it is clear from figure 7 that the strengths reached by both the lime-RHA
specimens and those of cement-RHA are very similar.
STATISTICAL ANALYSIS OF qu AS RESPONSE VARIABLE

Table 5 shows the experimental matrix developed in this research. In addition, such a matrix enables easy visu-
alization of the experiment combinations in order to help the statistical analyses. The table displays the qu
obtained as response variable for the four controllable factors crossed.
The ANOVA presented in Table 6, performed on the qu results, showed that the effects of the controllable
variables: A − γd, B − RHA content, and D – curing type are statistically significant. It was not possible to
determine the statistical influence of the controllable factor C – CL content on the strength data, for the range
of contents investigated in the research, because its p value is greater than 0.05.
In addition, the interactions considered statistically significant were A*B, A*D, and B*D, as highlighted
in Table 6. As mentioned previously, the interactions between 3 and 4 controllable factors were used to
estimate the mean squared error because they are commonly not significant in the experiment.26–28
It should be noted that the presence of Ca(OH)2, provided by the inclusion of CL, is essential for the
occurrence of pozzolanic reactions between lime and RHA even though the levels investigated in this experi-
ment have not been significant. This means that the lime content cannot be excluded from the mixture.
Figure 8 displays the main effects plot for the analyzed independent variables, where comparisons about the
magnitudes of main effects can be made. The small magnitude of the lime content effect to the qu in comparison
to the other main effects analyzed can be observed in the figure.

JournalEDT 2020
TABLE 6
ANOVA
Source Degrees of Freedom MS F Value p Value Significative
A: γd, kN/m 3
2 15.515 91.46 0.000 YES
B: RHA content, % 2 52.077 307.00 0.000 YES
C: CL content, % 2 0.018 0.11 0.899 NO
D: Curing type 2 83.302 491.07 0.000 YES
A*B 4 1.104 6.51 0.000 YES
A*C 4 0.218 1.29 0.288 NO
A*D 4 1.540 9.08 0.000 YES
B*C 4 0.138 0.81 0.524 NO
B*D 4 4.030 23.76 0.000 YES
C*D 4 0.054 0.32 0.865 NO
Error 48 0.170
Total 80
FIG. 8
Main effect plots for qu.
Figure 9 shows the interaction plot matrix of the four studied factors. An interaction plot is a plot of means
for each level of a factor with the level of a second factor held constant. Interaction plots were useful for judging
the presence of interaction among the controllable factors. Because all the lines showed to be parallel one to
another, it is verified that the response variable, at any factor level, does not depend upon the level(s) of other
factors. Parallel lines in an interaction plot indicate no interaction.
In addition to statistical significance, the pairwise multiple comparisons of means (MCM) were made. The
MCM allow the assessment of the practical significance of differences between means. The underlined pairs of
means presented in figure 10 are not statistically different.
The MCM procedure indicates that increasing the values of γd results in significant strength gains for the
three levels analyzed; this behavior was likewise observed with the variations of RHA content. It means that each
level of the said independent variables are statistically different from one another. With regard to lime content,
neither one of the CL contents employed showed significant differences between themselves in the response
variable. As for the curing type, it has been found that curing the specimens for 7 days at 40°C is statistically
equivalent to curing for 28 days at 23°C.

JournalEDT 2020
FIG. 9 Interaction plots for qu.
FIG. 10 Multiple comparisons of means for qu.
By changing the temperature of curing from 23°C to 40°C for specimens cured for 7 days, the increase in the
strength results is highly significant. Extending the curing period from 7 days to 28 days showed the same effect.
On the other hand, the difference between curing at 40°C or for 28 days could not be verified. This means that
both curing types achieve statistically equal results.
According to Rojas and Cabrera,32 different factors can influence the kinetics and the quantities of the
hydrated phases produced by pozzolanic reactions. Curing temperature is the most important factor because
it influences the stability and the transformation of the hydrates. Metakaolin (used in Rojas and Cabrera’s32
research) and RHA (used in our research) have similar chemical contents. Both materials have more than
90 % of sum of SiO2 and Al2O3. Rojas and Cabrera32 have showed that specimens cured at 20°C have a slower
rate of reaction than specimens cured at 60°C, suggesting that lime consumption increases with rises in temper-
ature. For longer curing periods (180 days), lime is fully absorbed.32 According to Al-Mukhtar, Lasledj, and
Alcover,33,34 in their research, the total quantity of lime added was consumed after 28 days at 50°C and after
90 days at 20°C. The authors observed that there is a good correlation between the lime consumption and the
amount of CAH formed because of reactions. Therefore, pozzolanic reaction rate can be estimated from the lime
consumption, which is temperature dependent.

JournalEDT 2020
Therefore, it is not necessary to extend curing periods of the soil-ash-lime blends in regions where higher
ambient temperatures are easily reached (40°C or even above), as is the case in tropical countries such as Brazil,
India, Indonesia, Thailand, north of Australia, central portion of Africa, much of Southern and Central America,
because temperature acts as a catalyzer for the pozzolanic reactions. It is not the intent of this article to promote
the artificial increase of soil temperature in order to accelerate the curing process; rather, its intent is to raise
awareness of this phenomenon so that it may be used to one’s advantage when working with higher natural soil
temperatures. These findings directly affect road constructions because it means less time required for highway
interdiction during ground improvement works.
DURABILITY RESPONSE OF SOME SELECTED SPECIMENS

Durability is an important parameter for the base and subbase of pavements and thus was examined here as this is
a potential application for the proposed material. Durability tests were performed for varying CL and RHA
percentages, as well as γd of the specimens at 7 days of curing time in both temperatures (23°C and 40°C).
Specimens cured for 7 days at 40°C were shown to statistically have the same strength as the ones cured for
28 days at room temperature. Thus, durability tests were performed only for specimens cured for 7 days.
The wetting-drying cycles were carried out according to ASTM D559/D559M-15, Standard Test Methods for
Wetting and Drying Compacted Soil-Cement Mixtures,35 to determine the accumulated loss of mass (ALM) of
FIG. 11
Durability tests of some
selected specimens (A)
cured for 7 days at 23°C,
(B) cured for 7 days at
40°C.

JournalEDT 2020
studied blends. Such a standard allows the evaluation of mass losses after wetting-drying cycles. Each cycle begins
when specimens are placed underwater for 5 h at 23°C ± 2°C. Then, they are oven-dried for 42 h at 71°C ± 2°C.
Lastly, using a force of approximately 13 N, specimens are brushed 18 to 20 times.
Figure 11 illustrates values of ALM versus number of wetting-drying cycles for the two curing temperatures
for 7 days of curing. As presented in this figure, the higher ALM values occurred for two specimens molded with
10 % of RHA content for both curing temperatures. Increasing the RHA content is an appropriate alternative if an
increase in durability properties is required. In addition, higher values of γd and CL content cause a decrease in
ALM rates.
As stated by United States Army Corps of Engineers,36 the maximum allowable ALM, after 12 wetting-
drying cycles, is 11 % for granular materials, whereas the maximum value according to Portland Cement
Association37 is 14 % for soils classified as A-3 and stabilized with cement. Therefore, all ranges of porosities
and volumetric binder content tested in this study are adequate for both recommendations.
Concluding Remarks
From the results and analysis of tests described before, the following concluding remarks can be stated.
• An environment-friendly binder, made of two agricultural-industrial residues (RHA and CL), and blended
with a poorly graded fine sand, might be an alternative to enhance soil properties in regions where these
residues are produced. The substitution of portland cement by a binder made of residues is an important
advance to sustainability in geotechnical engineering.
• Rice cultivation regions usually do not have soils with good geotechnical properties. Therefore, the appli-
cation of this RHA + CL binder to bases or subbases of pavements can improve local road conditions,
which are usually very deteriorated because of intense traffic during harvest seasons.
• The use of adjusted porosity/volumetric binder index (η/Biv0.28) has been proven to predict the qu for
compacted sandy soil-RHA-CL, allowing the unification of RHA and CL contents in a single index.
• Larger values of RHA and CL contents and lower values of porosity represent better geotechnical properties
of blends, in other words, larger values of qu.
• The results showed that curing temperature acts as a catalyzer and higher temperatures accelerate pozzo-
lanic reactions between RHA and CL, improving blends’ parameter of strength.
• The ANOVA showed that the controllable factors γd, RHA content, and curing type are statistically
significant in the qu results (response variable). The greatest performance could be achieved by employing
the highest γd and the highest content of RHA independent of the amount of CL chosen. However, it should
be pointed out that the presence of Ca(OH)2 is essential for the occurrence of the pozzolanic reactions.
Thus, at least a minimum amount of lime is required.
• Regarding the curing type, the engineer can choose between curing at higher temperatures (40°C) for a
shorter period of time or for a longer period (28 days) at 23°C. Thus, the decision can be made according to
the temperatures reached at the construction site or the time available to complete the ground improve-
ment. Adopting shorter times, when curing is performed at higher temperatures, is warranted because high
temperatures are easily achieved in tropical countries, such as Brazil. Also, when it comes to road
construction, this design decision allows a faster release to traffic, reducing the inconveniences caused
by highway interdictions.
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JournalEDT 2020
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Journal of Testing and Evaluation

doi:10.1520/JTE20180763 / Vol. 48 / No. 3 / 2020 / available online at www.astm.org

Helena Batista Leon,1 Mariana da Silva Carretta,1 Maurício Birkan Azevedo,1

Statistical Analysis of the Influence of

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SiO2 93.6 3.10

Note: ND = not detected.

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Molding and Curing of Specimens

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14.5 10, 20, 30 5, 8, 11 7-23; 7-40; 28-23

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Unconfined Compression Tests

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Independent Variable Number of Levels Real Levels

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INFLUENCE OF THE η/Biv0.28

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Unconfined Compressive Strength, MPa

14.5 15.5 16.5

RHA, % RHA, % RHA, %

CL, % CL, % CL, % CL, % CL, % CL, % CL, % CL, % CL, %

qu ðMPaÞ = 3.05 × 104 ðη=Biv 0.28 Þ−3.60 ½R2 = 0.78 (5)

qu ðMPaÞ = 1.19 × 105 ðη=Biv 0.28 Þ−3.60 ½R2 = 0.80 (6)

qu ðMPaÞ = 1.17 × 105 ðη=Biv 0.28 Þ−3.60 ½R2 = 0.65 (7)

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STATISTICAL ANALYSIS OF qu AS RESPONSE VARIABLE

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Source Degrees of Freedom MS F Value p Value Significative

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FIG. 9 Interaction plots for qu.

FIG. 10 Multiple comparisons of means for qu.

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DURABILITY RESPONSE OF SOME SELECTED SPECIMENS

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