Journal of Materials Research and Technology 33 (2024) 7123–7135

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Journal of Materials Research and Technology

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

Effect of the loss on ignition on the unconfined compressive strength of

residual clays from Bogotá-Colombia stabilized with cement
Liliana Carolina Hernández García **, Henry A. Colorado Lopera *
CCComposites Laboratory, Universidad de Antioquia UdeA, Calle 70 No. 52-21, Medellín, 050010, Colombia

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

Keywords: Organic matter in rock aggregates, such as subgrade, sand, and gravel, originates from the decomposition of
Clayey waste organic remains, including plants and domestic waste. The method used to measure the organic matter content in
Soil cement aggregates for infrastructure projects is known as Loss on Ignition (LOI) in which the difference in weight before
Pavements
and after calcination is considered the percentage of loss due to oxides, carbon, nitrogen, phosphorus, and sulfur
Clays
Marginal waste
derived from the organic material. This study compares the compressive strength of three clayey wastes sourced
Soil stabilization from Bogotá, Colombia, each with different organic matter contents measured by loss on ignition (LOI), mixed
Unconfined compression strength with varying cement contents. A total of 153 cylindrical samples were manufactured using a monotonic
Plasticity index compression compaction technique with different cement and water dosages. Monotonic compression is a type of
test in which a load is applied continuously from zero until failure occurs, without any unloading. The physical
characterization was reviewed with plasticity limits, specific gravity (Gs), methylene blue index (M.B.I.),
chemical composition with X-ray Fluorescence (XRF) X-ray diffraction (XRD) and SEM micrographs. Through
multivariate statistical techniques, compressive strength was correlated with the Water/Cement ratio and the
Cement/Residue ratio, resulting in a function that facilitates calculation of cement dosage and water content. The
study identified that the response surfaces of clayey residue types exhibit tighter concavity as organic matter
content increases, indicating a narrower range for determining optimum moisture content with higher LOI. This
experimental investigation aims to explore the feasibility of incorporating clayey waste enhanced with hydraulic
cement into materials for infrastructure construction, thereby reducing reliance on natural resources. However,
the results indicate that these materials can be utilized in constructing sustainable pavements by applying more
rigorous moisture measurement and control techniques to the mixtures. This approach compensates for the use of
waste materials by reducing the need for landfills, saving production energy, preventing pollution from material
extraction and exploitation, and decreasing gas emissions that contribute to global climate change.

1. Introduction silica fume, acai ash [3] (see Table 1). There is also abundant research
regarding the use of waste materials in soils and construction materials
The excessive exploitation of natural resources is the main cause of [4–6]. although the composition are very much dependent of the loca-
the global crisis, and the biggest challenge facing the current generation tion of the research. Despite efforts to utilize local raw materials in the
is the reduction of emissions and carbon footprint on the planet [1]. The region [7,8], technical specifications often limit their use in most
’Bend the Trend 2024′ report compares the increase in material con- infrastructure projects [9], although there are large scale successful
sumption over the last 50 years, rising from 8.4 to 13.2 tons per year per cases particularly when the use of waste materials is included in the
inhabitant worldwide. This represents an average growth of 2.3% per regulation [10,11].
year. The construction sector is one of the main sources of environ- Materials such as compressible clays, organic clays, and peat are
mental degradation, with natural resource consumption estimated at strata that typically need to be removed and discarded at construction
106.6 billion tons per year and less than 5% of waste being reused [2] sites due to their high organic matter content, tendency to swell, ab-
such as fly ash, rubber fiber, the reclaimed asphalt pavement (RAP), sorption capacity, deformability, and low strength [12]. These cohesive

* Corresponding author.
** Corresponding author.
E-mail addresses: [email protected] (L.C. Hernández García), [email protected] (H.A. Colorado Lopera).

https://doi.org/10.1016/j.jmrt.2024.11.081
Received 9 October 2024; Received in revised form 7 November 2024; Accepted 9 November 2024
Available online 10 November 2024
2238-7854/© 2024 Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
L.C. Hernández García and H.A. Colorado Lopera Journal of Materials Research and Technology 33 (2024) 7123–7135

materials fall under the category of marginal construction and demoli- To identify the relationship between the cement content, the additive
tion waste, constituting approximately 11% of all construction and de- used and the plasticity index of the soil-cement mixtures of the publi-
molition waste [13]. This marginal waste is often utilized in backfilling cations in Fig. 2, the cluster analysis was carried out to classify the ob-
for landscaping purposes, especially in areas affected by mining activ- servations into homogeneous groups with respect to the three variables.
ities or road and track conditioning [14]. The variability of resistance is due to the plasticity of the material, the
To enhance the mechanical properties of fillings containing clayey or consistency of the mixture (whether it is fluid or dry), the additive or
marginal waste, various mixing technologies involving hydraulic ce- addition and the cement content. It is observed that in four groups,
ments, glass, ash, and other manufactured wastes have been studied mixtures with low cement contents, low fluidity and little plasticity
[15–23]. These physical and chemical modifications aim to reduce ab- register higher strength to unconfined compression, as shown in Fig. 3.
sorption, swelling, and the effects of organic materials present in the There are several modeling methods for predicting the strength of
waste, such as the inhibition of proper hydration in cement-based mix- mixtures between clay materials and hydraulic cement. However,
tures, reduced strength, and decomposition caused by biological several authors use linear models because of their precision [26,27]. In
mechanisms. However, the stabilization of clay wastes with cement re- the literature review, it was identified that the authors focus on
quires studying different variables that affect its strength, such as measuring the development of long-term resistance (28, 60, and 90
moisture content, material plasticity, and density. These factors must be days). However, the building regulations for roads indicate that traffic
carefully balanced in the cement content of the mixture during the must be opened 7 days after the mixture is installed [28,29]. For this
design process [24,25]. reason, this research focuses on measuring and predicting strength at
Between 2014 and 2024, nearly 40,000 articles on the mixtures of that age. Regardless of whether hydraulic cement develops higher
clay soils with cement have been indexed in major scientific publication long-term strengths, the state at 7 days will define its performance under
databases. The peak in publications occurred in 2023, and this trend is service load [30].
continuing to grow. As illustrated in Fig. 1, Engineering comprises the The American Concrete Institute in its report 230.1R-09 [55], es-
largest share of publications at 33%, followed by Earth and Planetary tablishes the guidelines for the design, construction, and inspection of
Sciences at 19%, and Materials Science at 15%. soils with cement mixtures, which are ratified by the Portland Cement
Fig. 2 presents the results of unconfined compressive strength (UCS) Association’s (PCA) soil stabilization guide [56]. In both documents, soil
in kPa from various scientific publications featuring clay materials cement is defined as a compact mixture of soil, Portland or hydraulic
mixed with hydraulic cement and other strength-enhancing additives. cement, and water used for various pavement and foundation applica-
The most utilized dosages range between 7% and 15%, resulting in tions. It also classifies soil cement into four categories: Cement Modified
compressive strengths between 1 MPa and 6 MPa. Soil (CMS), Cement Stabilized Subgrade (CSS), Cement Treated Base

Table 1
Unconfined compressive strength of soils mixed with cement and admixtures.
USCS AASHTO Admixture Liquid limit Plasticity index Cement Content Strength (kPa) Fuente

CL-ML A-7 Only Cement 65.9% 25.0% 6.0% 350 [31]

CL A-7 Nanosilica 43.0% 23.0% 0% 686.5 [32]
SP A-3 Silica sand 0.0% 0.0% 8.0% 701 [33]
CL A-6 Nanosilica 36.3% 14.1% 7% 1231 [34]
CL-ML A-6 Cement II 24.4% 4.2% 9.0% 1300 [35]
GW A-1-A Cement bound material 0.0% 0.0% 4.5% 1600 [36]
CL A-7 Nanosilica 42.4% 15.3% 15% 1800 [37]
CH A-7 Only Cement 138.0% 95.8% 4% 2000 [38]
GW A-1-A RAP_BG2 0.0% 0.0% 5.4% 2700 [36]
CH A-7 Oil Shale ash 72.0% 42.0% 6.0% 2750 [39]
SP A-3 Silica_sand2 34.0% 0.0% 6.0% 2900 [40]
SC A-4 Char 32.0% 9.0% 20% 3800 [41]
CH A-7 Rubber fiber 137.0% 91.0% 10% 4500 [42]
SC SC5 Fly ash 15.3% 6.1% 9% 4800 [43]
SC A-2-6 NRL 21.0% 13.0% 5.0% 5500 [44]
SC A-4 GGBS_1 27.6% 9.3% 7.50% 5740 [45]
GW A-1-A Reclaimed asphalt pavement 0.0% 0.0% 9.0% 5800 [46]
SC A-4 Only Cement 27.6% 9.3% 12% 5830 [45]
SC A-6 Nanosilica 30.0% 13.5% 15% 5851.4 [47]
SC A-2-6 Reclaimed asphalt pavement 23.0% 18.0% 7.0% 6000 [48]
SC A-4 Silica fume 15.3% 6.1% 9% 6400 [43]
CH A-7 Fly ash 88.0% 54.0% 25% 6500 [49]
CL A-7 Graphene oxide 41.5% 19.6% 15.0% 6505 [50]
SC A-4 Sugarcane bagasse ash 15.3% 6.1% 9% 6510 [43]
CL A-7 PVA 44.8% 20.2% 15% 7200 [51]
CL A-6 Titanium slag 33.2% 14.2% 30.0% 8000 [52]
SM A-7 Acai ash 45.0% 27.0% 9.5% 8200 [43]
SC A-4 Ground granulated blast-furnace slag 27.6% 9.3% 10% 8316 [45]
SC A-4 Only Cement 15.3% 6.1% 10% 10500 [43]
SC A-4 Acai ash 15.3% 6.1% 9% 11000 [43]
CL A-7 Only Cement 52.8% 25.9% 25% 1300 [53]
SC A-3 Silty 39.4% 0.0% 25% 1450 [53]
CL A-7 Only Cement 61.8% 34.3% 17% 1000 [47]
CL A-7 Only Cement 53.0% 25.0% 22% 683 [48]
CL A-7 Soil organic 42.0% 25.0% 9% 5000 [12]
CH A-7 Phosphogypsum 111.9% 67.9% 21.70% 100 [54]
CH A-7 Phosphogypsum 83.6% 48.6% 16.50% 110
CL A-6 Phosphogypsum 38.5% 15.2% 9.50% 460
ML A-7 Phosphogypsum 44.0% 12.5% 10.30% 400

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Fig. 1. Papers published in Scopus and Science Direct from 2014 to 2024.

Fig. 2. Unconfined compressive strength from different scientific publications in 2023–2024.

(CTB), and Full Depth Reclamation (FDR). water. This material can be prepared on-site or in the plant, and its
Cement-modified soil (CMS) is characterized by being composed of compressive strength at seven days can range between 2000 and 4000
fine natural soils of low plasticity, low doses of hydraulic cement, and kPa [57].
water. Its function is to improve workability, dehydrate the soil, and FDR (Full Depth Reclamation) is known as the recycled material
increase the speed of construction in rainy areas. This type of treatment from deteriorated pavements obtained after the process of milling,
enhances the load-bearing capacity of the soil by providing a permanent crushing, and pulverizing the running surface of the asphalt pavement
modification. In this case, the material does not require a maturation and the underlying layers, which could be granular or subgrade bases.
period for the application of loads, so the design strength at 7 days is This scarified material is mixed with cement and water, producing a
very low, ranging between 690 and 2000 kPa. homogeneous and stabilized compact layer with good structural ca-
On the other hand, Cement Stabilized Subgrade (CSS) is a material pacity, as well as the economic and environmental benefits of waste
with a slightly higher cement content than CMS. Its purpose is to be part recycling [58].
of the pavement structure and improve the CBR bearing capacity, shear In that order, the PCA recommends a model for the design of soil-
strength, compressive strength, and shrinkage/swelling deformations cement mixtures based on soil characterization, compaction percent-
after several wetting and drying cycles. age, and unconfined compressive strength [59]. On the other hand, the
The Cement Treated Base (CTB) is a mixture of manufactured soil American Association of State Highway and Transportation Officials
that meets a design gradation, a higher cement content than CMS, and (AASHTO) defines the design methods for soil-cement mixtures based on

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Fig. 3. Non-hierarchical cluster of soil cement with the variables PI, Cement and additive content and unconfined compression.

the moisture-density ratio tests (T134) [60], wetting and drying tests more sustainable infrastructure.
(T135) [61], and freezing and thawing test (T36) [62].
The purpose of the soil cement design is to enhance the mechanical 2. Materials and methods
characteristics of the soil in its natural state. However, there are stan-
dards that must be met to obtain a cement-stabilized base and subbase. The materials used for this modeling were clay wastes sourced from
AASHTO, in conjunction with the General Contractors Association the Colombian capital, as shown in Fig. 4. The first waste is produced
(AGC) and the American Road and Transportation Builders Association from the washing of sedimentary gravels. Its physical classification is
(ARTBA), developed a Guide Specification for producing Pozzolanic fine clayey sand with a maximum nominal size of 0.18 mm and 10% by
Stabilized Mix (PSM) bases. This guide is now used by the Federal weight of kaolinite clay, classified as fine non-plastic clayey sand (NP)
Highway Administration [63], and it is summarized in the following according to the Unified Classification System (UCS). The second waste
table. is obtained from mining deposits related to the exploitation and washing
The European standard BS EN 14227–15:2015 has similar standards of sedimentary sands, sourced from the surface of sludge pools. Its
to those shown in Table 2. It regulates the dosage, construction, and mineralogical classification corresponds to kaolinite clay with a plas-
quality control of hydraulically bound soil mixtures for roads, aero- ticity index (PI) of 35. The third waste is used as a filling material from
dromes, and other traffic areas. This European standard covers soil deep excavations in infrastructure projects and corresponds to kaolinite
stabilization using one or a combination of cement, fly ash, hydraulic clay with the presence of diatoms, registering a plasticity index (PI) of
road binder, lime, and blast furnace slag [78]. 60.
Case studies report that road construction using natural soils mixed The physical and chemical characterization of the three wastes in-
with cement increases vehicular load capacity, enhances resistance to dicates that each has distinct silica, Loss on ignition from 110 ◦ C to
water softening through chemical bonding of particles, and reduces 1000 ◦ C, and liquid limit contents that are proportional to each other, as
traffic stresses, thereby providing a stronger platform [79–81]. Addi- shown in Table 3.
tionally, it can reduce the thicknesses required in the pavement structure Where LL is the Liquid Limit, PL is the Plastic Limit, PI is the Plas-
[57,81]. Incorporating marginal waste into the design and construction ticity Index, Gs is the Specific Gravity, I.A.M. is the Methylene Blue
of pavements can reduce the excessive exploitation of natural resources, Index (meq/100 g s), LOI is the Loss on ignition from 110 ◦ C to 1000 ◦ C,
as well as emissions and carbon footprint. For this reason, in this and NP stands for Not Plastic.
experimental work, the unconfined compressive strength results of Early high-strength hydraulic cement (ART) was used to manufac-
clayey waste from excavation and stone aggregate mining, mixed with ture the specimens. Its chemical composition is detailed in Table 4 and
Portland cement, are modeled to compare the effect of organic matter compared with the chemical requirements of Portland cement according
content on the mix design. to ASTM C150/C150M − 22 [74], which corresponds to Portland
Pavements constructed with cement treated soil are 11% cheaper Cement Type I.
than those with traditional structures. The results of this research,
applied to pavement construction, enhance material performance at a 3. Experimental design
lower cost. The reuse of clay waste reduces the need for transporting
granular material, resulting in a solution that can be replicated widely During the experiment, 153 cylindrical samples were manufactured
and applied to numerous materials. This method can reduce carbon and tested for compression after 7 days of curing, following procedure
emissions by approximately 20%, thanks to decreased material transport D1633-17 [75]. The samples taken from each waste source were sub-
and a 32% reduction in pavement thickness. Overall, these changes jected to a drying treatment at 110 ◦ C (230 ◦ F), followed by a crushing
translate to a smaller carbon footprint, shorter construction times, and a process and finally a grinding process, until a homogeneous dust was

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Table 2
Test procedures for base and subbase mixtures with cement.
Property Standard Test Method Regulations

Gradation %Material passing no. 4 > 50% Sieve analysis of fine and Coarse Aggregates1 ASTM C136/
AASHTO T27 [64]
Abrasion resistance Sufficient particle resistance to resist degradation and Resistance to degradation of small size coarse aggregate by ASTM C131/
breakage during construction and under repeated traffic abrasion and impact on the Los Angeles machine AASHTO T96 [65]
loads.
Max: 35%
Plasticity LL<25% PI<4% Liquid limit, plastic plasticity index of soils ASTM D4318 [66]
Soundness of aggregates Sodium Sulfate, Max: 12 Soundness of aggregates by use of Sodium Sulfate or ASTM C88/AASHTO
Magnesium Sulfate, Max:18 Magnesium Sulfate T104 [67]
Harmful components Sand Content, min.: 15%. Equivalent value of soil sand and fine aggregates (indirect ASTM D2419 [68]
Organic matter content, max.: 2% measure of the clay content of aggregate mixtures)
Compressive strength Min: 2500 kPa (7 days) Manufacture and curing of soil-cement compression and ASTM D1632 [69]
Max: 4500 kPa (7 days) bending test specimens in the laboratory ASTM C593 [70]
Freeze-thaw durability Mass losses, Max: 14% Freeze and thaw testing of compacted soil-cement mixtures ASTM D560 [71]
Maximum dry density and According to service load Moisture-density ratios of soils and soil-aggregate mixtures ASTM D698
optimal moisture content using a 2.49 kg (5.5 lb) rammer and a 305 mm (12 in.) drop (estándar) [72] o
or ASTM D1557
Moisture-density ratios of soils and soil-aggregate mixtures (modificado) [73]
using a 10 lb. (4.59 kg) rammer and an 18 in (457 mm) drop
Compact density Min: 95% density maximum Soil density in place by the sand cone method ASTM D1556 [74]
Density and unit weight of the soil laid using the rubber ASTM D2167 [75]
balloon method
Volumetric stability Swelling, max: 5% One-dimensional expansion, contraction and pressure ASTM D3877 [76]
increase of soil-lime mixtures
Resilient module According to service load Resilient module of unbonded granular base/subbase AASHTO T274 [77]
materials and subgrade soils

Fig. 4. Origin of each of the selected samples a) Waste 1 from washing gravel mining, b) Waste 2 from the sludge pool from the rock sand washing and c) Waste 3
from the filling with material from deep excavations in the city of Bogotá.

obtained that passes through a 200-mesh (75 μm) sieve (see Fig. 5). stored in the curing booth (see Fig. 6).
Unlike traditional and standardized methods for compacting sam- Three samples of each waste type were produced for each dosage,
ples, a specially designed mold was used in this investigation, which using four different cement contents and four different water contents.
complies with the dimensions required by ASTM D1632 [69]. With a Unconfined compression tests were conducted in accordance with ASTM
diameter of 72 mm and a height of 145 mm, a height/width ratio of 2 is D4219-11. After seven days of curing, the sample moisture, dry density,
achieved. Compaction was performed using a hydraulic press applying a and maximum compressive strength were recorded.
maximum load of 200 kN. After compaction, the cylinder was removed The chemical characterization of the materials was performed using
and stored in a curing booth for 7 days at a temperature of 23 ◦ C and a X-ray fluorescence (XRF) MLQFRX010. For scanning electron micro-
relative humidity of 98%. Unlike the traditional method, this approach scopy (SEM) characterization, the samples were fractured, dried for 24 h
reduces the effect of porosity on the test results [82]. at 60 ◦ C in an electric oven, and then pulverized to facilitate analysis.
The manufacturing process of the sample involves mixing the spec- The samples were coated with a thin film of gold to enhance conduc-
ified dosage (by weight) of clay residue, hydraulic cement, and water tivity. The equipment used was a JEOL JSM 6700R in a high vacuum
until a homogeneous mixture with consistent kneading is achieved. mode and its calibration is carried out with the automatic adjustment
Because clay materials tend to form lumps and clods when mixed with package.
water, this effect is mitigated by applying the water using a spray that The tests were conducted using a Malvern Panalytical X-ray
disperses it evenly. Once the mixture is ready, it is introduced into the diffractometer (XRD) Model Empyrean 2012, equipped with a Pixel 3D
mold and tamped with a blunt-point rod of 3/8″ diameter, applying 35 detector and a Co source (λ = 1.790307) at 40 kV and 40 mA. The
taps in a spiral pattern from bottom to top [76]. The piston is then placed goniometer was set to Omega/2 theta mode with a platform configu-
inside the mold, and the sample is compacted using a hydraulic press, ration of Reflection Transmission Spinner, rotating at 4 rpm. The step
starting with the top layer until a load of 200 kN is reached. The collar is size was 0.01◦ , with a time per step of 50 s. A ½◦ divergence slit and a 1◦
removed, the mold is rotated, and then the load is applied again to the anti-scattering slit were used. Phase quantification was performed using
underside. Finally, the sample is extracted, its mass is recorded, and it is High Score Plus software with the Rietveld method and the ICSD FIZ

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Table 3
Physical and chemical characterization of waste.
Waste LL PL PI Gs I.A.M. Composition (%)

SiO2 Al2O3 Fe2O3 CaO MgO LOI (110-100 ◦ C) Σ

1 21% – NP 2.33 3.40 80.1 8.9 4.4 0.18 2.42 4.0 100
2 59% 24% 35% 2.28 8.20 65.1 16.6 7.92 0.09 3.49 6.8 100
3 90% 24% 66% 1.76 10.00 62.0 16.7 3.7 0.7 3.2 13.7 100

Table 4
Oxide content (%) measured by X-ray fluorescence.
CaO SiO2 Al2O3 SO3 Fe2O3 MgO P2O5 LOI Σ

Cement 68.04 13.9 4.58 3.06 3.06 3.97 0.137 3.25 100
ASTM C150 ​ ​ 6 max. 3.5 max. 6 max. 6 max. ​ 1.1 max ​

Fig. 5. Sample Preparation, (a) natural drying, (b) kiln drying, (c) crushing, (d) abrasive charge for grinding.

Fig. 6. Processing of cylindrical specimens with a width to height ratio of 1:2.

Karlsruhe 2012-1 database, using rutile as the internal standard. Table 5 shows the composition of the phases of the materials, as
Data interpretation was carried out through multivariate analysis, defined by the diffraction curves presented in Fig. 7. A trend is observed
employing techniques and models that range from exploratory analysis in the variation of the chemical composition of the mixtures, where part
to the identification of patterns in multivariate data. The variables of the kaolinite clay is transformed into calcite and lime. Note how the
analyzed included cement content, water-cement ratio, dry density, organic matter content and variations in the chemical composition of the
porosity, void ratio, organic matter content, plasticity index of clay clay contribute to the formation of calcite. Contrary to the findings in the
residue, and compressive strength. literature review, the residue with the highest organic matter content
For the review of the interrelations between the variables, a signif- developed more calcite, while the residue with the lowest organic matter
icance level of 5% was adopted. The assumptions of normality, inde- content developed less calcite. It is initially deduced that the organic
pendence, multicollinearity, specification, and homoscedasticity were material retains the water necessary to form calcium bonds in the dry
also validated. consistency soil-cement mixtures.
Table 6 shows the chemical composition of each mixture. It is
4. Results observed that the formation of CaCO3 is proportional to the cement
content in the mix (see Table 7).
4.1. Chemical characterization Following the AASHTO T267 and ASTM D999 methodologies, the
organic content of the three soils was determined. This method quan-
Using X-ray diffraction (XRD) techniques, the crystalline materials tifies the oxidation of organic matter by exposing the sample in a furnace
and phase identifications of the wastes used in the mix design were for 6 h at 445 ◦ C. The organic content is expressed as a percentage of the
characterized. When compared with previously validated databases, mass of the dried soil, as shown in the table.
Fig. 7 illustrates the results of the samples, which showed the greatest On the other hand, the SEM micrographs reveal the transformation of
similarity to the wastes used. The graph highlights the distinctive peaks the clay mineral (see Fig. 8). Before mixing with hydraulic cement, the
of quartz (Q), kaolinite (K), and hydraulic cement components such as structure of the kaolinite clay is observed as slabs. After mixing and at
CSH, calcite (Ca6C6O18), and lime (Ca4O4). Compared to the samples the end of the curing period, these slabs are coated and agglomerated by
without hydraulic cement, the chemical reaction with kaolin results in calcite or calcium carbonate.
the formation of CSH gel, inversely proportional to the organic matter
content.

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Fig. 7. XRD for mixtures with different clay wastes, waste 1 (4609), waste 2 (4610) and waste 3 (4617).

4.2. Mechanical characterization S), and different water contents measured as the ratio of the mass of
water to the mass of the dry sample or soil (W/S).
A dataset of 153 unconfined compressive strength measurements (in In the graphical description of the variables shown in Fig. 9, an
MPa) was collected, using three types of clayey wastes with varying inversely proportional relationship between LOI and strength is identi-
organic matter contents (LOI), different cement contents measured as fied. That is, higher organic material content correlates with lower
the ratio of the mass of cement to the mass of the dry sample or soil (C/ compressive strength. Conversely, higher cement content is associated

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Table 5 Table 7
Semi-quantification by X-ray diffraction - Qualitative. Mass Loss on ignition by organic matter content, ASTM D999 method.
Quartz Kaolinite Calcite Lime Waste Initial mass Final mass % Mass Loss on Ignition (LOI)
Si6O6 Al2Si2O9H4 Ca6C6O18 Ca4O4
1 100.0 92.55 7.45
Waste 1 81% 19% ​ ​ 2 100.0 90.48 9.52
Waste 1 þ Cem 74% 19% 7% ​ 3 100.0 83.22 16.78
Waste 2 62% 38% ​ ​
Waste 2 þ Cem 57% 23% 18% 2%
Waste 3 54% 46% ​ ​
Waste 3þCem 52% 25% 23% C W C W
​
MPa SC = − 1.05035 − 23.06507 + 19.19359 + 74.15867 •
S S S S
C2 W2
with increased strength, while a higher water-cement ratio leads to − 85.56135 − 95.656
S S
reduced strength. The distribution of the strength data is platykurtic and Eq 1
skewed to the right, indicating that it is not normally distributed.
Therefore, an automatic transformation of the variable was applied to Where MPa SC represents the strength of sandy wastes, C/S is the mass of
validate the model, given by (UCS_T = UCS0.2120646), using R Studio. cement divided by the mass of dry soil, and W/S is the mass of water
Where LOI represents loss to ignition by organic material, Strength divided by the mass of dry soil. With 75% reliability, the response sur-
refers to the unconfined compressive strength in MPa, Cement/Soil de- face is characterized by the following statistically valid model:
notes the cement content in the mixture by weight, and Water/Cement is
C W C W
the water-cement ratio of the mixture. MPa CL = − 1.0732 − 3.7341 + 9.4205 + 25.1071 •
To identify any multicollinearity between the variables, the matrix S S S S
shown in Fig. 10 was reviewed. It reveals correlations between LOI and C2 W2
− 6.6910 − 16.2704 Eq 2
density, LOI and water content in the mixture, voids and porosity, and S S
density and water content in the mixture. Only untransformed UCS data
Where MPa CL represents the resistance of clay wastes with medium to
were used for this plot to validate the multicollinearity of the initial data
low plasticity, C/S is the mass of cement divided by the mass of dry soil,
before developing the model.
and W/S is the mass of water divided by the mass of dry soil. With 95%
On the other hand, there is little to no correlation between cement
reliability, the model for Sample 3, known as high plasticity clay with
content and the other variables. Strength (MPa) shows a proportional
LOI = 9.52, is given by the following equation:
relationship with cement density and content, while it has an inversely
proportional relationship with the void ratio (e), porosity (n), water C W C W
MPaCH = − 0.99815 − 5.89264 + 5.88862 + 10.2887 •
content in the mixture (W_S), organic matter content (LOI), and water- S S S S
cement ratio (W_C). C2 W2
+ 19.07801 − 6.12125 Eq 3
Multicollinearity in a statistical model suggests eliminating variables S S
with factors greater than 0.6 or replacing them with a single variable
that represents them. In this case, note that density is collinear with the Where MPa CH represents the resistance of high plasticity clay wastes, C/
void ratio and porosity (n > 0.6), which, in turn, are collinear with the S is the mass of cement divided by the mass of dry soil, and W/S is the
water content of the mixture ratio (W_S). The latter is related to the mass of water divided by the mass of dry soil. To predict the optimal
water/cement ratio (W_C). To meet the assumption of non- cement content for the mixture, the following model was validated, with
multicollinearity, the water/cement ratio (W_C) is selected as the a residual error of 0.02147 at 151 degrees of freedom, an R2 of 0.8185,
dependent variable to represent density, water content (W_S), porosity and an adjusted R2 of 0.8136. The statistical F-value is 170.2 with 4 and
(n), and empty ratio (e). Additionally, the cement content (C_S) is chosen 151 degrees of freedom (Fisher-Snedecor distribution), and the p-value
as an intervening variable, while unconfined compressive strength is < 2.2e-16.
(UCS) is selected as the response variable. C = 0.05645 − 1.67756 LOI− 1.233872
− 0.15252W0.2794664
Where LOI represents the loss on ignition by organic material, UCS is
the unconfined compressive strength in MPa, Density is the dry density + 0.25113 σ MPa 0.2120646 Eq 4
of the sample, e is the void ratio, n is the porosity, W_C is the water/
Where C is the mass of cement, LOI is loss on ignition, W is the mass of
cement ratio, and C_S is the cement content in the mix. To establish the
water, and σ MPa is the resistance in MPa. After model validation, the
variability between mix design models with different clayey wastes, the
assumptions of normality, homogeneity, constant variance, and residual
response surface was constructed using R Studio, as shown in Fig. 11.
variability were verified.
This indicates that as the LOI content and plasticity increase, the range
After reviewing the assumptions, it is concluded that the model is
of optimum moisture content required to achieve higher compaction
statistically valid (see Table 8). Fig. 12 shows a graph comparing the
and strength becomes narrower.
laboratory-measured responses with the predicted responses using
With 95% reliability, Residue 1, known as clay sand with LOI = 7.45,
Equation No. 4. As an example, it is used to calculate the cement content
exhibits a response surface characterized by the model:
of a mixture required to achieve a strength of 4.5 MPa, with varying LOI
values as shown in Table 9:
According to this research, water content depends on the mixing
conditions. For dry consistencies, it is recommended to use 3% of the LOI

Table 6
XRF chemical composition of waste mixtures with hydraulic cement.
CaCO3 SiO2 MgO Al2O3 Si K Ca Fe Σ

Waste 1 17.20 45.70 0 3.87 10.74 0.64 18.55 3.29 100

Waste 2 18.49 41.84 0 6.09 18.93 0.80 8.55 5.31 100
Waste 3 21.03 46.4 0.46 5.93 18.41 0.59 5.67 1.53 100

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Fig. 8. SEM micrograph of wastes before and seven days after mixing. CSH hydration phases: (1) Portlandite Ca (OH)2, (2) Tobemorite Si2O7H6, and (3) Ettringite.

value. However, given real-world limitations, it is recommended to recycled asphalt, and others, due to their absorption, granulometry, and
determine the in-situ moisture content and the moisture reduction once chemical composition.
mixed with cement, as this may facilitate calculating the mix moisture
factor needed to achieve the results from the equation. 5. Discussion
The preparation of the mixtures includes only clay residues, Type I or
High Early Strength cement, and water. The results differ from those of The clayey wastes used in this research are kaolinite-rich materials
mixtures containing additional ingredients such as ash, Nanosilica, with varying proportions and origins, which affect their plasticity and,

Fig. 9. Graphical description of box and whisker diagrams between the variables of the experiment.

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Fig. 10. Multicollinearity matrix between variables.

Fig. 11. Response surface of the three samples.

consequently, their adsorption capacity. Residue 1 is classified as fine

Table 8
sand with a minor proportion of kaolinite clay, while Wastes 2 and 3,
Validation of model assumptions made in R Studio.
due to their plasticity index and liquid limit, are classified as high
Supposed Model P-value Validation compressibility clays, and therefore, are considered marginal wastes. All
Homoscedasticity Goldfeld-Quandt 0.9995 Not rejected three materials exhibit low activity according to the methylene blue
Normality Kolmogorov-Smirnov 0.8188 Not rejected index, indicating low swelling capacity and low chemical instability
Variance Anova 2.2e-16 Rejected
[83]. This aligns with the characteristics of kaolinite clays.
Independence Durbin-Watson 0.35553 Not rejected
Specification Reset test 0.1316 Not rejected
It is known that the porosity (n) and void ratio (e) of soil-cement
mixtures affect the ultimate strength. However, by using the

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Fig. 12. Graph of actual responses and predicted responses with equation (4) model.

the compressive strength results range from lower to higher values

Table 9
depending on the cement content. Given the involvement of three
Application of equation (4) with different LOI.
wastes with different compositions and physical characteristics, the
LOI 4 6 8 10 12 dispersion of results is more pronounced. However, through statistical
Water (3%LOI) 12% 18% 24% 30% 36% transformations, it is feasible to construct a model that accurately cap-
σ (Mpa) 4.5 4.5 4.5 4.5 4.5 tures the variances among the three materials.
Cement 1% 12% 17% 20% 21% When comparing the results obtained in this research with those
from other publications (Table 1), similar trends can be observed.
monotonic compaction method, it was possible to minimize their However, the characterization of materials and cement differs. Soils
impact, resulting in more satisfactory modeling outcomes. improved with gravel and sand exhibit higher strength compared to
The wastes mixed with Portland cement showed a good development waste that is solely clayey. The type of cement, lime content, and the
of hydrated calcium as evidenced by X-ray diffraction and SEM micro- compaction method used for the sample are also factors that influence
graphs. However, the higher the quartz content, the higher the uncon- the result.
fined compressive strength. This indicates that the LOI content directly The key variables in the mathematical model are the water content in
affects the mix design and in turn the water content. the mix, the LOI content of the material, the cement content, and the
A waste with higher organic matter content requires a higher cement density of the mix. During the manufacturing stage, special care must be
content in the mix to achieve higher strength. The response surfaces taken with the application of the optimum moisture content. The
showed that compressive strength was higher with the lowest LOI con- response surfaces for the three materials revealed a more pronounced
tent (7.45), while the waste with the highest LOI content (16.78%) concavity for those with high plasticity and high LOI content. If the
achieved only a third of the strength of the sample with the lowest LOI. water dosage is altered during the manufacturing or construction
This confirms that the higher the LOI content, the lower the unconfined stage—due to excess soil moisture, rain, or dehydration from high
compressive strength. temperatures—resistance should be compensated by increasing the
The concavity of the response surfaces indicates that the optimum cement content.
moisture range becomes narrower as the LOI increases. It is well known This may explain why laboratory-designed mixtures often show
that the disposal and final management of marginal soils with high variations in resistance when measured on-site. For sandy materials,
compressibility and high organic matter content generate additional variations in water content in the mix do not significantly affect
costs in pavement construction. It is important to note that their reuse strength. However, for cohesive materials with high plasticity and high
implies higher costs in cement stabilization and requires stricter mois- LOI content, strength is achieved only within a narrow range of opti-
ture control. In regions with fluctuating moisture conditions, specialized mum water content. A mixture with high moisture content tends to be
machinery and equipment must be available on site to achieve a ho- cohesive and viscous, while a mixture with low water content can
mogeneous mixture and ensure greater precision in adding the optimal become overly dry. In both cases, strength deteriorates more rapidly
moisture to the mix. Once installed and compacted, it is recommended compared to sandy or low plasticity materials.
to work in short sections and cover it with the next pavement layer as Moisture variation in the mix can be compensated for by increasing
soon as possible to avoid alterations in curing due to moisture variability the cement content, ensuring that the design strength is achieved during
in the area or climate conditions. the construction process. Both moisture content and cement content are
described in Equations (1)–(3), which characterize the behavior of the
6. Conclusions response surfaces for the three materials.
To consolidate the three intervening variables in the response vari-
The graphical exploration of the results reveals significant variance able, a linear correlation model was validated to calculate the cement
in strength as a function of the LOI content of the material. Additionally, content required to achieve the design strength in pavement structures,

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interests or personal relationships that could have appeared to influence 10.3390/polym15143145.
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