land

Article
Clay Fraction Mineralogy and Structural Soil Attributes of Two
Soil Classes under the Semi-Arid Climate of Brazil
Thaís Cristina de Souza Lopes 1 , Jeane Cruz Portela 1 , Rafael Oliveira Batista 1 , Diego José da Costa Bandeira 1 ,
Isaque de Oliveira Leite 1 , Luirla Bento Ramalho 1 , Joaquim Emanuel Fernandes Gondim 1 ,
Joseane Dunga da Costa 2 , Marcelo Tavares Gurgel 1 , Carolina Malala Martins Souza 1 ,
Eulene Francisco da Silva 1 , Edivan Rodrigues de Souza 3 , Fábio Henrique Tavares de Oliveira 1 ,
Neyton de Oliveira Miranda 1 and Francisco Vanies da Silva Sá 1, *

1 Department of Agronomic and Forest Science, Federal Rural University of the Semi-Arid—UFERSA,
Mossoró 59625-900, Brazil
2 Department of Engineering and Technology, Federal Rural University of the Semi-Arid—UFERSA,
Pau dos Ferros 59900-000, Brazil
3 Agronomy Department, Federal Rural University of Pernambuco, Recife, Pernambuco 52171-900, Brazil
* Correspondence: vanies_agronomia@hotmail.com or vanies@ufersa.edu.br; Tel.: +55-(83)9-9861-9267

Citation: Lopes, T.C.d.S.; Portela, J.C.;
Batista, R.O.; Bandeira, D.J.d.C.; Leite,
I.d.O.; Ramalho, L.B.; Gondim, J.E.F.;
Costa, J.D.d.; Gurgel, M.T.; Souza,
C.M.M.; et al. Clay Fraction
Mineralogy and Structural Soil
Attributes of Two Soil Classes under
the Semi-Arid Climate of Brazil. Land
2022, 11, 2192. https://doi.org/
10.3390/land11122192
Academic Editor: Zhi-Hua Shi
Received: 24 September 2022
Accepted: 30 November 2022
Published: 3 December 2022
Publisher’s Note: MDPI stays neutral
with regard to jurisdictional claims in
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iations.
Copyright: © 2022 by the authors.
Licensee MDPI, Basel, Switzerland.
This article is an open access article
distributed under the terms and
conditions of the Creative Commons
Attribution (CC BY) license (https://
creativecommons.org/licenses/by/
4.0/).
Abstract: Mineralogical studies are incipient and necessary in the Apodi Plateau, Brazil. This study
aimed to evaluate the interrelationship between the mineralogy of the clay fraction and its structural
and chemical attributes and to differentiate two important pedo-environments in the semi-arid region
of northeastern Brazil (Ferralsol and Cambisols of the Apodi Plateau-RN) using the multivariate
technique. We evaluated the interrelationships between mineralogy and the structural and chemical
attributes of the soil and differentiated between agroenvironments. We collected soil samples from
six profiles in diagnostic horizons of the Ferralsols and Cambisols. In the mineralogical analysis of
the clay fraction, X-Ray Diffraction was used to identify mineral peaks of clay and iron oxides. The
physical and chemical properties of the soils were determined. The multivariate statistical technique
was applied to process the data. The clay minerals identified were hematite, goethite, kaolinite, and
illite. The principal component analysis allowed for the separation of environments according to soil
density, Fed and Mg2+ for developed soils, and potassium, weighted average diameter, microporosity,
total organic carbon, sodium, the sum of bases, calcium, total porosity, aeration, potential acidity,
and Feo discriminated developing soils. This study revealed that the clay fraction influenced the
structural attributes of the soil according to the degree of soil development. Two profiles presented
atypical situations: High contents of crystallized iron in Cambisols and illite peaks in Ferralsolos.
These mineralogical results are not commonly found in the literature, highlighting the potential for
further studies. The answers concerning the mineralogy of semiarid soils in Brazil and the world
show similarity.
Keywords: crystalline forms; atypical Cambisols; Brazilian drylands
1. Introduction
The Apodi Plateau covers 2146 km2 between the states of Ceará and Rio Grande do
Norte. This vast geomorphological unit has a flat relief with dominant slopes of <2% [1].
Moreover, the region has karst activity with soils derived from the Jandaíra formation [2],
determining morphogenetic processes that are decisive in the dynamics and evolution of
the landscape [3]. The Jandaíra formation belongs to the post-rift sequence of the Potiguar
Basin and is part of the Apodi group [4]. It rests on the sandstones of the Açu formation [5],
and in some areas, the karst features of the Jandaíra formation are covered by neogeneous
sediments from the Barreiras group [6].
This formation of the Cretaceous period (80–110 million years) consists of marine
carbonate sediments, characteristic of shallow and agitated water environments, in addition

Land 2022, 11, 2192. https://doi.org/10.3390/land11122192 https://www.mdpi.com/journal/land

Land 2022, 11, 2192 2 of 17

to deposited bioclastic calcarenites and calcilutites, forming a carbonate platform that

covered the entire emerged portion of the Potiguar Basin during the Turonian and the
Mesocampanian ages [7,8]. The shallow marine carbonate rocks of the Jandaíra formation
have been subject to significant variations in permeability over time due to various fracture
events and calcite cementation [7].
Soils formed on carbonate rocks show high levels of calcium carbonate and pre-
dominant minerals such as calcite and dolomite, which are typical of arid and semi-arid
regions [3,9]. Cambisols are the predominant soi class in the Brazilian semi-arid region
(Apodi Plateau-RN), even though Ferralsols, Argisols (Acrisols), and Chernosols (Cher-
nozems) are also identified [1,2,10]. Among soil attributes, the mineralogical composition
is one of the most important features since it influences physical and chemical phenomena
and is related to soil formation, offering indications about the degree of soil development
and the advance of weathering [11].
The mineralogy of the soil clay fraction varies depending on the soil parent material
and soil position in the landscape [12]. In highly weathered soils (Ferralsols), typical of
tropical regions, kaolinite peaks and iron and aluminum oxides (hematite, goethite, and
gibbsite) predominate. Iron and aluminum oxides have different degrees of crystallinity
and are evaluated according to mineral groups based on the iron content (Feo/Fed ratio);
they are extractable forms of iron, Feo quantification of Iron in amorphous forms extracted
by oxalate and Fed- quantification of iron in crystalline forms, extracted by dithionite-
citrate-sodium bicarbonate [12,13]. The Feo/Fed ratio is an important soil weathering
indicator, with values below one indicating developed soils [14]. However, Cambisols have
a predominant mineralogical composition of 2:1 clays (illite, vermiculite, smectites, and
micas) formed by the process of bisialitization that is typical of low to intermediate soils
(about pedogenetic evolution) in the semi-arid region of Brazil [1].
From this perspective, the mineralogy of the clay fraction is closely related to phys-
ical and chemical soil properties, influencing the soil structure due to the formation and
maintenance of aggregates and soil density [15]. In addition, cohesion and adhesion forces
influence mechanical processes that govern macroscopic soil properties and are determined
by the processes of flocculation and dispersion, which depend on molecular interactions at
the particle level [16,17]. Moreover, soil mineralogy influences phosphate sorption phenom-
ena and geochemical processes, e.g., nutrient cycling and the soil availability of nutrients
and heavy metals [18–20].
The literature contains several studies on the clay fraction conducted with various
types of soils [1,18,21–23]. However, there are still gaps to be filled to better understand
clay mineralogy, especially in arid and semi-arid regions. Studies of this nature can im-
prove planning activities for low-carbon agriculture, predicting the effects of land use
associated with weathering and pedogenesis. These studies are essential for soil surveys,
ecological/biogeochemical modeling, and decision-making for sustainable actions. There-
fore, this study aimed to evaluate the interrelationship between the mineralogy of the
clay fraction and its structural and chemical attributes and to differentiate two important
pedo-environments in the semi-arid region of northeastern Brazil (Ferralsol and Cambisols
of the Apodi Plateau-RN) using the multivariate technique. The hypothesis stated that the
mineralogy of the clay fraction would influence the structural attributes according to the
degree of development of the studied soil classes.

2. Materials and Methods

2.1. Study Area and Sample Collection
This study was carried out in two Settlement Projects (SP) in the Apodi Plateau micro-
region of the Potiguar West mesoregion, State of Rio Grande do Norte, Brazil (Figure 1).
The studied settlements were called “Terra da Esperança” (Governor Dix-Sept Rosado) and
“Moacir Lucena” (Apodi). The climate of the region is classified as BSw’h (hot semi-arid)
according to Köppen [24], and the natural vegetation is the Caatinga dry forest biome.
Land 2022,Land 2022, 11, x FOR PEER REVIEW
11, 2192 3 of 17 4 of 18

Location
Figure 1.Figure map of the
1. Location mapstudy area
of the of Governador
study Dix-SeptDix-Sept
area of Governador Rosado and Apodi
Rosado andinApodi
the northeast
in the northeast
of Brazil.of Brazil.
Land 2022, 11, 2192 4 of 17

The soils of the studied areas are classified as Cambisols and Ferralsols according
to [25] and to the World Reference Base—WRB [26] published by the Food and Agriculture
Organization of the United Nations—FAO. The research was carried out in six Agroecosys-
tems (Table 1), two Ferralsols, and four Cambisols by investigating different diagnostic
horizons (Bi/Cambisols and Bw/Ferralsol) of the soil class profiles in both SP.

Table 1. Uses and classification and location of the environments.

Profile Horizont (m) Soil Class/WRB Land Use Settlement

P1 Bw (0.48–1.20) Ferralsol Recovering—RC
P2 Bi (0.15–0.54) Haplic Cambisol Lake—L Moacir Lucena
P3 Bw (0.25–0.97) Ferralsol Reserve—R
P4 Bi (0.08–0.37) Haplic Cambisol Native Forest—NF
Terra da
P5 Bi (0.07–0.22) Haplic Cambisol Colective—CC
Esperança
P6 Bi (0.10–0.42) Haplic Cambisol Agroecological—A

Soil samples were collected for laboratory analysis in the diagnostic horizons of the
Cambisol (Bi) and Ferralsol (Bw) classes, with deformed and undeformed structures [27].
The incipient B horizon (Bi) is a sub-surface diagnostic horizon underlying the A, Ap, or AB
horizons and shows physical and chemical modifications in a not very advanced degree,
although sufficient for developing color and structural units. In contrast, the Ferralsols
B horizon (Bw) is a sub-surface mineral horizon that exhibits advanced weathering with
the transformation of easily changeable minerals, followed by intense desilication, base
leaching, and residual concentrations of 1:1 sesquioxide and clay minerals and weathering-
resistant minerals [25].
A deformed sample was collected from each diagnostic horizon, with the aid of a
shovel and tray, placed in plastic bags, identified, and sent to the laboratory. The soil
was air-dried, ground, and passed through 2 mm sieves to obtain fine air-dried soil for
measuring its texture and chemical and mineralogical attributes. The laboratory procedure
was performed in four replicates.
The undeformed samples, totaling ten samples for each horizon of the respective soil
profiles, were collected to determine the Ma (soil macroporosity), Mi (soil microporosity),
TP (total porosity and aeration), and BD (bulk density). For the extraction of the samples,
the horizons prior to the diagnosis were removed with the aid of a straight shovel. The
Uhland extractor and rings measuring 0.05 m in both height and diameter were used
for that purpose, resulting in impacts sufficient to promote penetration of the ring into
the ground. After collection, the rings were coated with aluminum foil and taken to the
laboratory to preserve the soil structure and moisture.

2.2. Soil Analyses

2.2.1. Physical Analyses and Aggregate Stability
The physical parameters presented in Table 2 were determined and subjected to
multivariate statistical analysis to assess their influence on the studied soil characteristics.
Furthermore, as a physical procedure, the clay fraction of the samples collected from the
diagnostic horizons was prepared for further mineralogical characterization. The separation
of the clay fraction from the other granulometric fractions was performed using chemical
dispersion (0.025 mol.L−1 sodium hexametaphosphate) and mechanical stirring (with a
“Wagner” agitator for 16 h). After each collection, the volume of each beaker was completed
with sodium carbonate solution at pH 10, thus maintaining the pH between 8 and 8.5. This
procedure was repeated until the clay fraction was totally removed [28].
The blocks extracted in the soil profiles were passed through 4 mm and −2 mm sieves,
thus preserving the structure of the aggregates. The aggregates retained in the 2 mm sieve
were placed in cans, after which the wet sieving method was employed [29]. Four 25 g
replicates were used for each profile. After pre-wetting, the samples were transferred to a
set of 4.76, 2, 1, 0.5, and 0.25 sieves in the vertical oscillator working at 42 oscillations per
Land 2022, 11, 2192 5 of 17

minute [30] and then taken to the oven at 105 ◦ C. Subsequently, the samples were placed
in an oven (105 ◦ C), and the aggregates were quantified. Based on the dry mass, the sand
fraction was discounted using a dispersing solution (NaOH mol.L−1 solution), and the
aggregate size distribution and geometric and weighted average diameters were obtained.

Table 2. Physical characteristics of soils with their respective methods and standards.

Physical Attributes Unity Method

Sand Total (2–0.05 mm) g.kg−1 Screening
Clay (<0.002 mm) g.kg−1 Sedimentation
Silt (0.05–0.002 mm) g.kg−1 Sedimentation
BD kg.dm−3 Volumetric ring
Mi 1 cm3 .cm−3 Tension table
TP 2 cm3 .cm−3 Tension table
Paeration cm3 .cm−3 Tension table
Ma cm3 .cm−3 Macroporosity = (TP − Microporosity)
WMD mm [29]
1 Microporosity soil was determined by the water content of the soil at a height value equal to 60 cm of water
(approximately a pore radius of 25 µm). 2 The volumetric rings were saturated for 48 h and weighed to determine
the total porosity. BD: bulk density; Mi: microporosity soil; TP: total porosity; Paeration : aeration porosity; Ma:
macroporosity soil; WMD: Weighted mean diameter.

2.2.2. Chemical and Mineralogical Analyses

The chemical attributes determined are shown in Table 3. The variables of TOC,
exchangeable Na+ , Ca2+ Mg2+ and K+ (H+Al), pH, and SB (sum of exchangeable basic
cations (K+ , Ca2+ , Mg2+ and Na+ ). Furthermore, the iron oxides were quantified to support
the mineralogical analysis of the collected soil samples. For this, three different analyses
were carried out in the diagnostic horizons of the studied soils.

Table 3. Chemical characteristics of soils and their respective methods.

Chemical Attributes Unity Method

TOC g.kg−1 Digestion of organic matter 1 .
pH Agitation of a soil-water suspension (1:5) for 2 h
Calcium (Ca2+ ) mg.dm−3 Titrometry 2 .
Sodium (Na+ ) mg.dm−3 Titrometry 2 .
Magnesium (Mg2+ ) mg.dm−3 Titrometry 2 .
Potassium (K+ ) mg.dm−3 Titrometry 2 .
Potential acidity (H + Al) calcium acetate 0.5 mol L−1
Atomic Absorption Spectrophotometry, with a
Fes g.kg−1
sulfuric attack.
Atomic Absorption Spectrophotometry, using
Fed g.kg−1
Dithionite-Citrate-Bicarbonate.
Atomic Absorption Spectrophotometry, using
Feo g.kg−1
ammonium oxalate.
1 The samples were crushed, which were passed through an 80-mesh sieve, then added potassium dichromate
and carried on a hot plate. Afterwards, orthophosphoric acid and distilled water were added, being titrated with
ferrous ammonium sulfate (0.05 M). 2 Determined using potassium chloride extractor, using ascorbic acid and
titrated with ethylenediamine tetra acetic acid (0.0125 M).

Sulfuric attack was initially carried out [31] to quantify the iron content present in the
secondary minerals (Fes). For this, about 0.5 g of air-dried fine earth was used in 75 mL
digestion tubes along with 20 mL of H2 SO4 (at a 1:1 ratio with deionized H2 O) by taking
the digester block to the temperature of approximately 180 ◦ C for one hour. For cooling,
50 mL of deionized water was added, and the material was filtered through blue strip filter
paper into 250 mL volumetric flasks [28].
Subsequently, the quantification of Fe in crystalline forms (Fed) was performed. For
this, 0.2 g of clay was weighed and placed in 50 mL centrifuge tubes. Then, 10 mL of the
Land 2022, 11, 2192 6 of 17

0.2 mol. L−1 citrate solution and 0.5 g of powdered sodium dithionite were added to the
tubes. Next, the tubes were taken to a water bath (at 50 ◦ C) for 30 min, after which the
tubes were removed, cooled at room temperature, and taken to the centrifuge at 2000 rpm.
Finally, the extract was placed in a 50 mL volumetric flask. All steps were repeated three
times. Then, the volumetric flask was filled with deionized water. A blank test containing
the reagents and the final extract was carried out in parallel to the analysis, and the iron
content was read with an atomic absorption spectrophotometer.
The iron content was determined by the oxalate method to quantify amorphous iron
forms (Feo). For this, 0.2 g of clay was weighed and placed in centrifuge tubes covered
with aluminum foil. Then, 10 mL of the “Tamm reagent” solution (0.2 mol.L−1 ammonium
oxalate + 0.2 mol.L−1 oxalic acid at pH 3) was added, after which the tubes were sealed and
taken to a horizontal shaker, where they were fixed parallel to the direction of movement
and agitated for two hours. Then, the samples were centrifuged for 10 min at 2000 rpm. The
final extract was transferred to 50-mL volumetric flasks and supplemented with deionized
water. A blank test containing the reagents was carried out in parallel to the analysis. The
extracts were also read with an atomic absorption spectrophotometer.

2.2.3. Mineralogical Analyses

The mineral peaks present in the clay fraction were identified by X-Ray Diffraction
(XRD) with a SHIMADZU diffractometer, model XRD—6000, using kα1 emission from
copper (Cu). The source potential was 40 kV, and the current was 30 mA. A scanning speed
with a step of 0.02◦ was applied every second. The scanning range (2θ) was established from
5 to 70◦ using the program X-Ray v. 1.0.0.37, and the minerals were identified according
to [32].

2.3. Statistical Analyses

After obtaining the data on the attributes with a deformed structure, expressed by the
mean of four repetitions in the laboratory, the data were subjected to statistical analysis
through multivariate analysis to detect the most sensitive attributes using the software
Statistica 7.0 [33]. Pearson’s Correlation Matrix (P ≤ 0.05), Factor Analysis, Principal
Component Analysis, and Cluster Analysis were used during this step. Pearson’s correla-
tion analysis was adopted for 19 variables to ensure that they showed sufficient minimal
correlations to justify their use in the data matrix.

3. Results
3.1. Physical and Chemical Attributes
Table 4 presents the average physical, chemical, structural, and mineralogical values
in soil classes for each diagnostic horizon. The sand fraction predominates in the surface
soil classes, except for profile 4. The explicit silt contents in the Cambissols (P4, P5, and P6)
indicate less weathered soils. The clay fraction increased in depth in all soil classes, except
profile 4 (Bi 0.08–0.37 m). The highest levels of iron (Fes) occurred in profiles 1 (Ferralsol)
and 6 (Cambisol). Soil density was higher in Ferralsols (P1 and P3). Profiles 2, 4, 5, and 6
(Cambisols) showed more excellent resistance to the action of the active agent’s water and
wind due to the higher values of WMD, as well as microporosity and total porosity of the
soil. To pH, all classes had an alkaline character, including the weathered ones (Ferralsol).
Total Organic Carbon (TOC) decreased in depth in all profiles. However, considering
low contents, higher in Cambisols. In general, occurred low levels of phosphorus (P),
low levels of potassium (K+ ), and no restrictions on sodium (Na+ ). The bases Ca2+ and
Mg2+ and the sum of bases were higher in Cambisols. The classes showed a eutrophic
character (V ≥ 50%). The highest values of potential acidity (H+Al) occurred in the Ferralsol
without restrictions.
Land 2022, 11, 2192 7 of 17

Table 4. Mean values of physical, chemical, structural and mineralogical attributes in soil classes,
Apodi Plateau, Rio Grande do Norte, Brazil.

Sand Silt Clay BD Mi Ma TP PA WMD pH TOC P K Na Ca Mg SB V% H+Al

Horizontes
(cm) 3 3 3 mg
g kg−1 g cm cm cm (%) mm g kg−1 cmolc kg
kg−1
Profile 1—Ferralsol
A (0–4) 660 87 253 1.60 0.27 0.14 0.41 9.40 0.94 7.24 4.80 7.19 0.47 0.03 4.30 3.80 8.60 81.47 1.96
AB (4–17) 492 92 416 1.61 0.39 0.04 0.43 15.30 0.96 6.68 3.73 2.56 0.31 0.03 3.10 3.10 6.54 71.12 2.66
BA (17–48) 371 81 548 1.85 0.20 0.13 0.33 10.50 0.98 6.28 7.84 2.67 0.10 0.04 3.30 2.60 6.04 71.29 2.43
Bw (48–120) 397 97 506 1.51 0.38 0.03 0.41 12.50 0.94 6.80 4.93 2.88 0.05 0.03 3.40 3.00 6.48 82.26 1.40
BC
382 148 470 1.60 0.39 0.05 0.44 14.10 1.95 6.58 1.77 2.25 0.05 0.02 2.50 3.80 6.37 82.90 1.31
(120–155+)
Profile 2—Cambissol
A (0–3) 653 96 251 0.72 0.30 0.07 0.37 15.20 1.85 7.64 6.23 4.56 0.42 0.08 7.10 3.30 10.90 89.65 1.26
BA (3–15) 415 135 450 1.16 0.20 0.21 0.41 21.10 1.89 6.75 3.20 2.14 0.32 0.04 4.90 3.30 8.56 79.74 2.17
Bi (15–54) 311 153 536 1.37 0.41 0.03 0.44 27.40 1.96 6.51 3.54 2.14 0.05 0.03 6.40 3.40 9.88 81.93 2.18
BC (54–75) 179 230 591 1.29 0.47 0.02 0.49 23.70 1.99 7.10 2.95 3.09 0.04 0.06 13.40 6.20 19.70 91.78 1.77
C (75–85+) 322 137 541 1.39 0.45 0.03 0.48 19.50 7.21 1.58 7.82 0.04 0.16 20.10 8.50 28.80 99.54 0.13
Profile 3—Ferralsol
A (0–7) 656 57 287 1.67 0.28 0.08 0.36 22.21 0.81 7.30 7.83 2.88 0.37 0.0 3.30 3.00 6.69 85.05 1.18
BA (7–25) 556 37 407 1.72 0.29 0.08 0.37 21.10 0.99 6.51 4.38 1.09 0.21 0.0 4.10 0.70 5.04 75.96 1.6
Bw (25–97) 444 44 512 1.62 0.35 0.09 0.44 20.00 0.99 6.33 4.38 2.56 0.13 0.0 4.60 0.30 5.06 77.92 1.44
BC (97–140+) 479 49 472 1.58 0.37 0.05 0.42 19.85 1.02 6.93 2.19 1.40 0.10 0.0 4.30 1.00 5.43 83.81 1.05
Profile 4—Cambissol
A (0–8) 489 174 337 0.96 0.53 0.08 0.61 27.32 1.76 7.06 32.10 1.50 1.15 0.28 24.30 0.15 25.88 100 0.00
Bi (8–37) 537 97 366 1.23 0.47 0.08 0.55 23.32 1.19 7.64 9.19 1.50 0.23 0.41 32.30 0.70 33.64 100 0.00
C (37–52) 642 106 252 1.31 0.38 0.08 0.46 18.89 1.36 8.58 5.81 2.50 0.21 0.32 24.80 3.70 29.03 100 0.00
R (52+) - - - - - - - - - - - - - - - -
Profile 5—Cambissol
A (0–7) 673 94 233 1.32 0.43 0.02 0.45 22.84 1.56 8.15 48.35 3.70 2.30 0.16 17.80 0.60 20.86 100 0.00
Bi (7–25) 569 151 281 1.35 0.42 0.06 0.48 21.16 1.18 8.48 9.18 0.90 0.41 0.21 15.80 1.30 17.72 100 0.00
Bi/C (25–50) 560 170 270 1.39 0.41 0.06 0.47 20.39 1.21 8.52 8.52 1.90 0.25 0.20 17.30 1.40 19.15 100 0.00
CB (50–200+) 536 182 282 1.42 0.43 0.03 0.46 21.15 1.49 8.48 5.00 2.50 0.18 0.21 15.80 1.20 17.39 100 0.00
Profile 6—Cambissol
A (0–4) 691 90 219 1.53 0.37 0.02 0.39 18.55 1.84 7.72 20.34 2.20 1.92 0.16 15.80 5.70 23.58 100 0.00
BA (4–10) 679 77 244 1.59 0.39 0.03 0.42 19.21 1.95 7.60 15.86 5.08 0.07 0.05 9.43 2.46 12.01 100 0.00
Bi (10–42) 587 115 298 1.48 0.40 0.03 0.43 19.69 1.44 7.29 5.27 3.40 0.84 0.15 12.30 1.60 14.89 100 0.00
BiC (42–70) 539 206 255 1.49 0.41 0.05 0.46 19.68 1.44 7.50 3.91 2.59 0.27 0.05 12.13 2.02 14.47 100 0.00
CB (70–76) 519 207 274 - 0.41 0.06 0.47 19.47 1.28 7.40 3.59 0.90 0.15 0.06 14.47 1.91 16.59 100 0.00
C (76–91+) 674 63 264 - 0.41 0.06 0.47 19.49 0.84 7.84 0.95 4.70 0.53 0.16 13.30 5.00 18.99 100 0.00
PA—Aeration porosity.

3.2. Mineralogical Attributes

The identification of the mineral peaks of the clay fraction allowed us to separate the
soil classes into two groups. One of the groups included developed soils belonging to the
Red-Yellow Ferralsol (P1), Haplic Cambisol (P2), and Yellow Ferralsol (P3) classes. The
other comprised developing soils (P4, P5, and P6), both classified as Haplic Cambisols
(Table 5).

Table 5. Mean values Fe2 O3 contents extracted by sulfuric attack, dithionite-citrate-bicarbonate and
ammonium oxalate, and the Feo/Fed ratio.

Fes Fed Feo Feo/Fed Clay

Profile/Horizont
g/kg
P1—Bw (Ferralsol) 13.31 2.89 0.54 0.19 506
P2—Bi (Cambisol) 7.81 2.08 1.65 0.79 536
P3—Bw (Ferralsol) 8.82 3.25 0.90 0.28 512
P4—Bi (Cambisol) 8.96 0.62 0.36 0.57 366
P5—Bi (Cambisol) 8.64 0.75 0.43 0.58 281
P6—Bi (Cambisol) 10.36 0.75 0.21 0.28 298
Fes—Iron by sulfuric attack; Fed—Iron by dithionite; Feo—Iron by oxalate; Feo/Fed: Feo/Fed ratio.
 P6—Bi (Cambisol) 10.36 0.75 0.21 0.28 298
Fes—Iron by sulfuric attack; Fed—Iron by dithionite; Feo—Iron by oxalate; Feo/Fed: Feo/Fed ratio.

The degree of crystallinity of iron oxides (Feo/Fed) ranged from 0.19 (Red-Yellow
Land 2022, 11, 2192 Ferralsol) to 0.79 (Haplic Cambisol). P3 (Yellow Ferralsol) showed the highest Fed content 8 of 17
(3.25 g.kg−1) among the studied soils. For the Feo content (amorphous iron), which ranged
from 0.21 to 1.65 g.kg−1, the mean value was 0.90 g.kg−1. P4 (Haplic Cambisol) had the
lowest Fed content (0.62 g.kg−1) among the studied soils. With regard to the Feo/Fed ratio,
The degree of crystallinity of iron oxides (Feo/Fed) ranged from 0.19 (Red-Yellow
most soil classes showed values below 1, corroborating their weathered characteristics.
Ferralsol) to 0.79 (Haplic Cambisol). P3 (Yellow Ferralsol) showed the highest Fed content
The XRD of the natural clay from the diagnostic horizons is shown in Figures 2 and
(3.25 g.kg−1 ) among the studied soils. For the Feo content (amorphous iron), which ranged
3. Among the clay mineral groups, Fe oxides (goethite and hematite), type 1:1 clay miner-
from 0.21 to 1.65 g.kg−1 , the mean value was 0.90 g.kg−1 . P4 (Haplic Cambisol) had the
als (kaolinite), and illite (2:1 − non-expansive clay mineral derived from mica) were ob-
lowest Fed content (0.62 g.kg 1 ) among the studied soils. With regard to the Feo/Fed ratio,
served in all studied soils.
most soil classes showed values below 1, corroborating their weathered characteristics.
The mineralogy of developed soils (Ferralsols) (Figure 2) is consistent with their evo-
The XRD of the natural clay from the diagnostic horizons is shown in Figures 2 and 3.
lutionary
Among thestage.
clayAccordingly, all profiles
mineral groups, showed
Fe oxides well-defined
(goethite kaolinite
and hematite), type(Ct)
1:1peaks, imply-
clay minerals
ing an advanced
(kaolinite), crystallization
and illite degree. In
(2:1 non-expansive claydeveloping soils (Cambisols)
mineral derived from mica) (Figure 3), mostin
were observed
profiles had two
all studied soils. expressive illite peaks (Il), implying fewer weathered minerals.

Land 2022, 11, x FOR PEER REVIEW 9 of 18

Figure
Figure2.2.XRD
XRD in in
thethe
natural clay
natural of the
clay diagnostic
of the horizons
diagnostic of the
horizons of most developed
the most horizons.
developed Ct:
horizons.
Kaolinite; Il: Illite; Gt: Goethite; Hm: Hematite; P1: Red-yellow Ferralsol—Bw; P2: Haplic Cambi-
Ct: Kaolinite; Il: Illite; Gt: Goethite; Hm: Hematite; P1: Red-yellow Ferralsol—Bw; P2: Haplic
sol—Bi; P3: Yellow Ferralsol—Bw.
Cambisol—Bi; P3: Yellow Ferralsol—Bw.

XDR XDR
Figure3. 3.
Figure in the clay
in the natural natural
of theclay of thehorizons
diagnostic diagnosticof thehorizons of thehorizons.
less developed less developed
2:1: 2:1-
horizons.
type mineral 2:1:clay;
2:1-type mineral clay;
Ct: Kaolinite; Ct: Gt:
Il: Illite; Kaolinite; Il: Illite;
Goethite; Gt: Goethite;
Hm: Hematite; P4: Hm: Hematite;
Haplic P4: Haplic
Cambisol—Bi; P5:
Cambisol—Bi;
Haplic Cambisol—Bi; P5: Haplic Cambisol—Bi;
P6: Haplic P6: Haplic Cambisol—Bi.
Cambisol—Bi.

3.3. Multivariate Statistical Analysis

The correlation matrix revealed significant correlations between the clay fraction and
the Fed and Feo contents and the properties of WMD, Mi, Ma, Mg2+ (H+Al), pH, and TOC.
The same was observed for Mi, Ma, Na+, Ca2+, Mg2+, SB, pH, and TOC (Table 6).
Land 2022, 11, 2192 9 of 17

The mineralogy of developed soils (Ferralsols) (Figure 2) is consistent with their

evolutionary stage. Accordingly, all profiles showed well-defined kaolinite (Ct) peaks,
implying an advanced crystallization degree. In developing soils (Cambisols) (Figure 3),
most profiles had two expressive illite peaks (Il), implying fewer weathered minerals.

3.3. Multivariate Statistical Analysis

The correlation matrix revealed significant correlations between the clay fraction and
the Fed and Feo contents and the properties of WMD, Mi, Ma, Mg2+ (H+Al), pH, and TOC.
The same was observed for Mi, Ma, Na+ , Ca2+ , Mg2+ , SB, pH, and TOC (Table 6).

Table 6. Correlation matrix between the variables of physical, chemical and mineralogical attributes
of the studied soils.

Atributes Clay Fes Fed Feo Feo/Fed TP P.A BD WMD Mi Ma Na+ Ca2+ Mg2+ K+ SB (H+Al) pH
Fes 0.10
Fed 0.88 0.29
Feo 0.75 −0.45 0.51
Feo/Fed −0.02 −0.77 −0.39 0.55
TP 0.06 −0.02 −0.33 0.32 0.64
P.A. 0.47 0.15 0.10 0.48 0.46 0.88
BD 0.53 0.36 0.84 0.17 −0.69 −0.67 −0.38
WMD −0.87 0.17 −0.65 −0.91 −0.41 −0.37 −0.65 −0.21
Mi −0.93 −0.20 −0.94 −0.71 0.17 0.06 −0.31 −0.73 0.80
Ma −0.98 −0.16 −0.84 −0.65 0.07 −0.04 −0.47 −0.48 0.79 0.86
Na+ −0.66 −0.24 −0.79 −0.57 0.27 0.14 −0.07 −0.80 0.57 0.88 0.54
Ca2+ −0.60 −0.31 −0.78 −0.47 0.36 0.20 0.00 −0.83 0.49 0.84 0.47 0.99
Mg2+ 0.86 0.05 0.94 0.69 −0.21 −0.28 0.05 0.82 −0.70 −0.96 −0.78 −0.89 −0.86
K+ −0.13 −0.19 0.18 −0.20 −0.47 −0.93 −0.93 0.58 0.40 0.01 0.14 −0.15 −0.18 0.26
SB −0.56 −0.35 −0.74 −0.45 0.35 0.14 −0.04 −0.79 0.48 0.81 0.43 0.98 1.00 −0.81 −0.12
(H+Al) 0.70 0.12 0.43 0.76 0.34 0.68 0.84 0.06 −0.83 −0.68 −0.63 −0.58 −0.50 0.50 −0.66 −0.53 1.00
pH −0.84 −0.23 −0.67 −0.62 0.12 −0.16 −0.45 −0.47 0.62 0.79 0.83 0.66 0.58 −0.72 0.11 0.56 −0.72 1.00
TOC −0.74 −0.16 −0.72 −0.62 0.22 0.07 −0.14 −0.70 0.54 0.84 0.66 0.88 0.83 −0.85 −0.17 0.81 −0.60 0.89
Clay; Fes—Iron by sulfuric attack; Fed—Iron by dithionite; Feo—Feo/Fed: Feo/Fed ratio; Iron by oxalate;
TP—total porosity determined; PA—Aeration porosity; BD—Bulk Density; WMD—weighted mean diameter;
Mi—Microporosity; Ma—Macroporosity; Na+ —sodium; Ca2+ —calcium; Mg2+ —Magnesium; K+ —Potassium;
SB: Sum of base; (H+Al): Potential acidez; pH: Hydrogen potential; TOC—Total Organic Carbon.

The variables of Feo/Fed, Paeration , and K+ did not correlate with the other variables
and were considered independent (Table 6). The high correlation observed corroborates
the adequacy of the data for using the cluster, principal component, and factorial analyses.
Two groups were formed when the reading was performed from right to left in the
vertical dendrogram obtained by cluster analysis (Figure 4), one of which was composed
of soil classes with developed pedogenesis (P1 and P3), both Ferralsols. These profiles
showed high dissimilarity and shorter Euclidean distances and were inserted into the first
group, indicating a distinction of the variables in relation to the data set.
The cumulative proportion of factors extracted from the 19 variables studied (factors 1
to 3) explained 91.14% of the total variability of the results (Table 7). F1 allowed for estimat-
ing the influence of expressive variables with significant factor loads in the differentiation
of the environments, especially clay, Fed, Feo, BD, WMD, Mi, Ma, Na+ , Ca2+ , Mg2+ , SB,
pH, and TOC. Factor analysis revealed that most causes of variation (F1 = 54.59%) are due
to the relationship between clay, Fe oxides, and structural attributes (Ma, Mi, WMD) and
soil chemistry (Na+ , Ca2+ , Mg2+ , SB, pH, and TOC). About F2, the variables that stood
out were Feo/Fed, TP, Paeration , and K+ (26.14%) (Table 7). F3 was the least expressive
parameter, with the lowest value of the selected attributes highlighting the Fes variable,
which describes the data related to iron oxides (10.41%). In addition, the sum of the cumu-
lative variances (F1 and F2) explained 80.73% of the variation and contributed the most to
distinguishing the studied environments (Table 7).
The WMD, K+ , BD, Fed, Mg2+ (H+Al), TP, and Paeration variables are close to the unit
circle (Figure 5A), meaning greater sensitivity in differentiating between environments
in relation to the other variables. According to the point cloud distribution (Figure 5B),
the most prominent variables in factor 1 are WMD, Mi, TOC, TP, Ca2+ , and Na+ . Factor 2
 oxalate; TP—total porosity determined; PA—Aeration porosity; BD—Bulk Density; WMD—
weighted mean diameter; Mi—Microporosity; Ma—Macroporosity; Na+—sodium; Ca2+—calcium;
Mg2+—Magnesium; K+—Potassium; SB: Sum of base; (H+Al): Potential acidez; pH: Hydrogen po-
tential; TOC—Total Organic Carbon.

The variables of Feo/Fed, Paeration, and K+ did not correlate with the other variables
Land 2022, 11, 2192 and were considered independent (Table 6). The high correlation observed corroborates 10 of 17
the adequacy of the data for using the cluster, principal component, and factorial analyses.
Two groups were formed when the reading was performed from right to left in the
vertical dendrogram obtained by cluster analysis (Figure 4), one of which was composed
included
of BD,
soil classes Fed,
with Mg2+ , clay,
developed (H+Al),(P1
pedogenesis andand
Paeration . Therefore,
P3), both Ferralsols.the significant
These profiles variables for
components
showed 1 and 2 (F1
high dissimilarity andand F2) Euclidean
shorter are thosedistances
that most and represent the studied
were inserted soils due to their
into the first
total accumulated
group, variance
indicating a distinction of in
therelation
variablesto
inthe totaltoofthethe
relation three
data set. factors (91.14%).

Figure
Figure 4. 4. Vertical
Vertical dendrogram
dendrogram of the distance
of the distance matrix bymatrix bybond
the single the single bond
grouping grouping
method. method. P1: Red-
P1: Red-
yellowFerralsol—Bw;
yellow Ferralsol—Bw; P2: Haplic
P2: Haplic Cambisol—Bi;
Cambisol—Bi; P3:Ferralsol—Bw;
P3: Yellow Yellow Ferralsol—Bw; P4: Haplic Cambisol—Bi;
P4: Haplic Cambisol—
Bi;
P5:P5:Haplic
Haplic Cambisol—Bi;
Cambisol—Bi; P6:P6:
Haplic Cambisol—Bi.
Haplic Cambisol—Bi.
The cumulative proportion of factors extracted from the 19 variables studied (factors
Table 7. Factorial axes extracted for soil attributes and their factor loadings, eigenvalues, total and
1 to 3) explained 91.14% of the total variability of the results (Table 7). F1 allowed for
cumulative variance.
estimating the influence of expressive variables with significant factor loads in the differ-
entiation of the environments, especially clay, Fed, Feo, BD, WMD, Mi, Ma, Na+, Ca2+,
Atributes Factor 1 Factor 2 Factor 3
Mg2+, SB, pH, and TOC. Factor analysis revealed that most causes of variation (F1 =
54.59%) are due to the relationship between clay, Fe−
Clay 0.90 and structural0.23
oxides, attributes (Ma, −0.07
Fes
Mi, WMD) and soil chemistry (Na+, Ca2+, Mg2+, SB, pH, −0.22
and TOC). About−F2, 0.26
the variables 0.94
Fed
that stood out were Feo/Fed, −0.92
TP, Paeration, and K+ (26.14%) (Table 7). F3 was−the
0.21least expres- 0.01
sive parameter, withFeo
the lowest value of the selected −attributes
0.70 0.51the Fes vari- −0.49
highlighting
able, which describes the data related to iron oxides 0.20
Feo/Fed (10.41%). In addition, the sum of the −0.54
0.80
cumulative variancesTP (F1 and F2) explained 80.73% 0.06 of the variation and0.93
contributed the 0.28
most to distinguishing the studied environments (Table
P. aeration −0.287). 0.89 0.34
BD −0.75 −0.66 0.02
WMD 0.76 −0.56 0.22
Mi 0.99 −0.03 0.02
Ma 0.83 −0.22 0.01
Na+ 0.91 0.18 −0.02
Ca2+ 0.87 0.26 −0.08
Mg2+ −0.96 −0.16 −0.22
K+ −0.03 −0.87 −0.45
SB 0.85 0.23 −0.14
(H+Al) −0.68 0.68 0.18
pH 0.84 −0.19 −0.12
TOC 0.90 0.08 0.02
Eigenvalues 10.37 4.97 1.98
Total Variance (%) 54.59 26.14 10.41
Accumulated Total Variance (%) 54.59 80.73 91.14
Clay; Fes—Iron by sulfuric attack; Fed—Iron by dithionite; Feo—Iron by oxalate; Feo/Fed: Feo/Fed ratio;
TP—total porosity determined; Paeration —Aeration porosity; BD—Bulk Density; WMD—weighted mean diameter;
Mi—Microporosity; Ma—Macroporosity; Na+ —sodium; Ca2+ —calcium; Mg2+ —Magnesium; K+ —Potassium;
SB: Sum of base; (H+Al): Potential acidez; pH: Hydrogen potential; TOC—Total Organic Carbon.
 Land 11,
Land 2022, 2022, 11, x FOR PEER REVIEW
2192 12 of 18 11 of 17

A B

Land 2022, 11, x FOR PEER REVIEW 12 of 18

A B

Figure 5. Cloud distribution of (A) variables in the correlation circle (B) points representing the
Figure 5. Cloud distribution of (A) variables in the correlation circle (B) points representing the
relates
relates betweenfactors
between 1–2 and
factors 1–2 andthe
theenvironments
environments studied.
studied. Similar
Similar colorscolors represent
represent profilesprofiles and their
and their
diagnostichorizons
diagnostic horizons and
and the
the discrimination
discriminationof of
soil attributes.
soil attributes.

B Mg2+ , and Na+ , highlighting

A The most important variables for F3 were Fes, Fed,
the interrelationship between iron oxides and structural attributes since they are part
of soils with different levels and types of clay, acting differently as aggregating agents
(Figure 6A). In addition, P2 (Haplic Cambisol) and P3 (Yellow Ferralsol) were sensitive
toFigure
Feo, whereas P1 (Red-Yellow
5. Cloud distribution Ferralsol)
of (A) variables in was sensitive circle
the correlation to Fes(B)
(Figure
points 6B). However,
representing the for
soils with
relates a less
between accentuated
factors 1–2 and thedegree, e.g., studied.
environments Cambisols (P4,
Similar P5,represent
colors and P6)profiles
(Figure
and6A),
their the
discriminating variables
diagnostic horizons and thewere TOC, WMD,
discrimination of soilMi, Na+ , and Ma (Figure 6B).
attributes.

A B

Figure 6. Cloud distribution of (A) variables in the correlation circle (B) points representing the
relates between factors 1–3 and the environments studied.

4. Discussion
The hierarchical analysis allowed the grouping of the studied soils into advanced
weathering (Ferralsols) and little-weathered categories (Cambisols), except for P2 (Cam-
bisol), which was grouped in P1 and P3 (Ferralsols). This can be explained by the fact that

Figure6.6. Cloud
Figure Cloud distribution of(A)
distribution of (A)variables
variablesininthe
thecorrelation
correlation circle
circle (B)(B) points
points representing
representing the the
relatesbetween
relates between factors
factors 1–3
1–3 and
and the
theenvironments
environmentsstudied.
studied.

4. Discussion
The hierarchical analysis allowed the grouping of the studied soils into advanced
weathering (Ferralsols) and little-weathered categories (Cambisols), except for P2 (Cam-
bisol), which was grouped in P1 and P3 (Ferralsols). This can be explained by the fact that
Land 2022, 11, 2192 12 of 17

4. Discussion
The hierarchical analysis allowed the grouping of the studied soils into advanced
weathering (Ferralsols) and little-weathered categories (Cambisols), except for P2 (Cam-
bisol), which was grouped in P1 and P3 (Ferralsols). This can be explained by the fact that
P2 (Cambisol) had a high amount of pedogenic iron oxides (Fed), similar to Ferralsols. This
finding is considered unusual in Cambisols of sedimentary origin and is little documented
in the literature, especially in the studied region.
The high Fed content in Cambisols could indicate developed soils even in conditions of
little pedogenesis, with the flat relief acting as an important factor in this process, similarly
to the study conducted in [34]. In another study, Girão et al. [35] analyzed the Fed levels
in Cambisol and Argisol profiles (Acrisols) in the Apodi Plateau and found that the Fed
values increased in Cambisols, suggesting variation in the degree of crystallinity. However,
greater homogeneity occurred in Argisols, which is characteristic of evolved soils.
Melfi et al. [36] point out that Cambisols have iron contents (Fe2 O3 ) lower than 5%
because they are poorly evolved. This low content is explained by the soil parent material
and the degree of soil pedogenesis. However, in the context of the Brazilian semi-arid
region, some soil classes have iron in the form of oxides. In addition, pedogeochemical
processes, such as sialferritization, justify iron incorporation into 2:1 clay mineral.
Girão et al. [35] argues that the presence of iron oxides in limestone-derived soils usu-
ally occurs in reddish clayey soils (5YR) and with oxide (hematite and goethite), kaolinitic,
and micaceous mineralogy. Anastacio et al. [37] pointed out that the mineralogy of the clay
fraction of Cambisols in the region of Minas Gerais (Brazil) consists mainly of maghemite
(Fe2 O3 ) and superparamagnetic goethite (FeOOH), in addition to kaolinite, smectite, and
smaller portions of anatase.
Ferralsols naturally show a greater presence of iron and aluminum oxides such as
hematite, goethite, and gibbsite, depending on variations in the parent material, the inten-
sity of weathering, and drainage conditions [38]. The oxidic constitution, virtually without
phyllosilicates, gives these soils a developed granular structure, low cation exchange capac-
ity, and excessive permeability, in addition to a relatively homogeneous color with reddish
or yellowish hues, horizon uniformity, and greater depths [39].
Correlations occurred between Fed, clay, and other structural attributes related to
soil aggregation (Mi, Ma, WMD, and Ca2+ ). Since soil texture contributes to stabilizing
and forming aggregates, soils with high clay contents favor aggregation since the clay
content favors particle adhesion, which, in turn, depends on complexing agents, silicate
minerals, Fe and Al oxides, ionic strength, pH, exchangeable cations, and phosphate
sorption [16,40]. Lu et al. [41] found strong and positive correlations between clay, iron
oxides (Fed), and pore sizes, mentioning that iron oxides and clay minerals (main kaolinite)
promote pedogenic cryptoporosity (<0.10 µm). In another study, Durn et al. [42] noted that
iron oxides were important in the aggregation of Cambisols in Croatia.
Moreover, although obtaining a low correlation between iron oxides and aggregation,
Yin et al. [43] pointed out that precipitated aluminum phosphates are important cementing
agents that stabilize soil aggregates. Mota et al. [40] highlighted that this aggregation
could be modified with soil preparation and biotic and abiotic factors. In addition to
cementing agents (iron and aluminum oxides), significant contributions of the carbon and
nitrogen cycles (aggregating agents) also promote the stability of soil aggregates (mainly
macroaggregates) [44].
In Brazilian subtropical regions, higher contents of crystalline iron were detected
in this soil class [35]. The levels of crystalline iron (Fed) vary according to the parent
material. Therefore, compared to basic rocks, sedimentary rocks show lower values of this
component [45,46]. Iron oxides (hematite and goethite) are correlated with soil structure and
aggregation, influencing water permeability and resistance to erosion [47]. Furthermore,
Fe2 O3 was observed at higher values in subsurface horizons than at the surface due to the
higher clay levels at those horizons, where the highest proportion of pedogenic Fe oxides
are concentrated.
Land 2022, 11, 2192 13 of 17

As for the structural attributes, soil texture was influenced by the more pronounced
presence of the clay fraction since soils with higher clay levels resulted in better aggregation,
increasing the contact between soil particles. The contrary was observed in sandy soils,
which hinder the formation of primary aggregates [48], with organic matter playing an
essential role in the formation of secondary aggregates [49].
The clay content supplies agglomerates of unitary particles resulting from the physical
attraction between particles and the action of cementing agents, e.g., iron oxides and
TOC [50,51]. Moreover, TOC is important for maintaining porosity and improving the
apparent soil density [52] since soil porosity directly influences the dynamics of organic
matter and the apparent density [53,54].
P3 (Ferralsol) had the highest soil density value, which could be due to the rearrange-
ment of particles since it corresponds to subsurface horizons where mineral translocation
occurs over short distances and the sand fraction predominates. Another factor that can
increase soil density is the presence of iron oxides. However, studies claim that these
factors have little influence but show effects when interacting with TOC and the soil clay
fraction [55,56].
The discriminating attributes in P4 (Cambissol) were Ca2+ and Na+ . This presence
of sodium is characteristic of semi-arid regions due to factors such as high evapotranspi-
ration [57], low rainfall [58], and anthropic interference [59]. Exchangeable calcium, on
the other hand, can be attributed to the parent material and the formation mechanisms
associated with pedogenetic processes, justifying the variability of soil classes in regions
with a limestone predominance. This was also reported in [60], which stated that those
soils show calcium accumulation and promote the formation of calcium or petrocalcic
horizons. Similar results were found in the research carried out in [2], in which high values
of exchangeable calcium were also detected.
Finally, P5 (Cambisol) showed low TOC and Mi values compared to the other classes.
This can be attributed to local climatic conditions and rainfall irregularity in association with
the type of vegetation of the semi-arid region [22]. In addition, the material of limestone
origin in P6 contributes to discriminating the values of structural attributes, e.g., WMD and
Mi, while providing Ca2+ and Na+ .
The low levels of iron oxides in the soil classes can be explained by sedimentary rocks
(Jandaíra Formation). This formation is characterized by sedimentary carbonate rocks with
small-scale, sub-vertical fractures [7], forming the largest exposed carbonate platform of
the Cretaceous on the Brazilian margin, where conspicuous outcrops form exposures up to
2 km wide [6]. Soils like these, derived from unconsolidated sediments, naturally have low
Fe contents and do not provide conditions for forming ferrimagnetic minerals [61].
Fe oxides can usually be distinguished into two types: Amorphous (Feo) or crystalline
(Fed) [62]. They have different degrees of crystallinity depending on the level of weathering,
parent material, and the position in the landscape [12,13], considerably influencing the
physical, chemical, and structural soil properties.
While Feo/Fed ratio values lower than one indicate more developed soils, values
above one indicate younger soils [63]. Thus, Ferralsols (weathered soils) have a low
Feo/Fed ratio, indicating higher iron contents in crystalline forms (Fed) due to greater
weathering [12,14,64]. The Feo content (amorphous iron) in P3 indicates greater pedogenic
development and fewer preserved characteristics of the parent material. In addition, the
presence of iron was visualized in the field in the form of concretions with a mean diameter
larger than 2 mm. These nodules are believed to be sources of information on pedogenetic
processes [65].
P4 had the lowest Fed content among the studied soils. It is believed that its condition
is characteristic of little-weathered soils and intrinsic to the parent material. Since Fe oxides
are important indicators of pedogenetic development, much of the Fe detected by Fe oxides
might be present as silicate clay minerals. In general, soils in semi-arid zones have low
Fe2 O3 levels, with few crystallized iron forms, mainly due to the climatic pattern and
Land 2022, 11, 2192 14 of 17

weathering processes [66]. In addition, those soils have poor drainage conditions, long
water deficit periods, and inefficient leaching [67].
In addition, the diffractograms showed well-defined kaolinite (Ct) peaks, indicating
that kaolinite is the dominant mineral in the studied soil classes, especially in Ferralsols. Ct
is generally formed from primary minerals (micas and feldspars) [68] in hot and humid
climates with intermediate mineral weathering and the partial removal of basic cations and
silicon [69]. Oliveira et al. [2] and Ferreira et al. [1] also point out that kaolinite was the
most common clay form found in the soils of the Apodi Plateau, whereas [70] stated that
kaolinite was the main mineral found in the clay fraction of weathered soils in the Amazon
basin. Similar results were described by [22] in Planosols.
Furthermore, the Cambisol class also showed kaolinite peaks (1:1) as well as iron and
aluminum oxides (hematite and goethite). Concerning this, [71] points out as a probable
hypothesis that muscovite will be present in the parent material (limestone rock), with
silica solubilization occurring under high pH conditions. In association with the balance
of the relationship between the activities of exchangeable bases (Ca2+ , Mg2+ , and K+ ), this
condition favors the formation of kaolinite even in the absence of pronounced leaching.
Furthermore, [72], in a study conducted in Cambisols of the Apodi Plateau, stated that
higher pH values favor silica dissolution and higher kaolinite contents. In addition, the
oxidation of 2:1 clay is not restricted to leached soils [21], as kaolinite formation can occur
in Cambisols.
Diffractograms also showed illite peaks (2:1 clay). While less common, type 2:1
clay minerals such as illite can be found in lower proportions in Ferralsols compared to
Cambisols [38]. The presence of type 2:1 clay minerals evidences the differentiation of the
class of Cambisols derived from limestone rocks abundant in the Apodi Plateau region [2].
As a mineral of the mica group, illite derives from the weathering of muscovite or
is inherited from calcareous parent materials [1]. Reference [2] described the presence of
2:1 illite and smectite clay minerals in Cambisols of the Apodi Plateau, corroborating the
present study. In addition, [23], studying soils of calcareous origin in the semi-arid region
of Morocco, pointed out that the mineralogy of the clay fraction was composed mainly of
illite, smectite (2:1), and kaolinite (1:1), varying depending on the parent material, climate,
and topography.

5. Conclusions
The present study investigated the mineralogical composition of the clay fraction of
Ferralsols and Cambisols in the Apodi Plateau, Brazil. The multivariate analysis allowed dif-
ferentiating agri-environments by indicating attributes with the most sensitive factor loads.
The structural attributes were valuable for discriminating Cambisols and the apparent soil
density and crystalline iron forms in Ferralsols. The clay fraction influenced the structural
attributes and varied according to the degree of development of the studied classes, corre-
lating with iron oxides. These iron oxides were positively correlated with soil aggregates,
acting as cementing agents in the studied soil classes. Under the semi-arid climate, both soil
classes showed clay fractions with the predominance of kaolinite (uncommon in Cambisols)
and a lower proportion of illite (uncommon in Ferralsols). One of the Cambisol profiles
(Profile 2) showed higher iron contents in the crystalline form, with kaolinite peaks and
iron oxides, constituting an improvement in the degree of development considering the flat
relief. The similarity of the formation factors help in the answers about the mineralogy of
soils in the semiarid region in Brazil and in the world. The study will be able to subsidize
the planning of programs and activities for development and carbon sequestration, effects
of land use on soils and pedogenesis, soil surveys and ecological/biogeochemical modeling
and decision-making in sustainable development actions.
Land 2022, 11, 2192 15 of 17

Author Contributions: T.C.d.S.L.: Conceptualization, Data curation, Formal analysis, Investiga-

tion, Methodology, Visualization, Validation, Project administration, Writing—original draft. J.C.P.:
Conceptualization, Investigation, Data curation, Methodology, Visualization, Validation, Project
administration, Resources, Supervision, Writing—original draft. J.E.F.G.: Data curation, Formal
analysis, Investigation, Software, Writing—original draft, Visualization, Validation, Writing—review
& editing. R.O.B.: Conceptualization, Investigation, Data curation, Methodology, Visualization,
Validation, Project administration, Resources, Supervision, Writing—original draft. E.F.d.S.: Data
curation, Methodology, Visualization, Validation, Writing—review & editing. C.M.M.S.: Data cura-
tion, Methodology, Visualization, Validation, Resources, Writing—review & editing. J.D.d.C.: Data
curation, Formal analysis, Investigation, Software, Visualization, Validation, Writing—original draft,
Writing—review & editing. D.J.d.C.B.: Data curation, Formal analysis, Investigation. L.B.R.: Data
curation, Formal analysis, Investigation, Writing—review & editing. F.H.T.d.O.: Methodology, Vi-
sualization, Validation, Resources, Writing—review & editing. M.T.G.: Investigation, Methodology,
Visualization, Validation, Resources, Writing—review & editing. E.R.d.S.: Investigation, Data cura-
tion, Methodology, Visualization, Validation, Writing—review & editing. N.d.O.M.: Methodology,
Visualization, Validation, Resources, Writing—review & editing. I.d.O.L.: Data curation, Formal
analysis, Investigation. F.V.d.S.S.: Investigation, Data curation, Methodology, Visualization, Valida-
tion, Resources, Supervision, Writing—review & editing. All authors have read and agreed to the
published version of the manuscript.
Funding: This study was financed in part by the Coordenação de Aperfeiçoamento de Pessoal de
Nível Superior—Brasil (CAPES)—Finance Code 001.
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: All other data are presented in the paper.
Conflicts of Interest: The authors declare no conflict of interest.

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