DOI: http://dx.doi.org/10.

1590/1678-992X-2016-0267
Soils and Plant Nutrition | Note

ISSN 1678-992X

Microstructural strength of four subtropical soils evaluated by rheometry:

properties, difficulties and opportunities
Patricia Pértile*, Dörthe Holthusen, Paulo Ivonir Gubiani, José Miguel Reichert

Federal University of Santa Maria – Soils Dept. – Av. ABSTRACT: The structural strength of soils has been extensively described by physical and
Roraima, 1000 – 97105-900 – Santa Maria, RS – Brazil. mechanical properties evaluated on the mesoscale for different soils and management condi-
*Corresponding author <[email protected]> tions. However, changes in the organization of the soil matrix at the microstructural level, which
can be obtained by rheometry, are still seldom used in soil mechanics. Our aim was to use the
Edited by: Silvia del Carmen Imhoff amplitude sweep test, a rheometry technique, to investigate the microstructural strength of four
subtropical soils (two Oxisols, an Ultisol and a Vertisol) and to discuss difficulties with respect
Received June 30, 2016 to the samples, water content, soil density and vertical force. The various rheological proper-
Accepted January 21, 2017 ties which reveal the soil microstructural strength were determined: deformation at the end of
the linear viscoelastic range, LVE range (γLVE), shear stress at the end of the LVE range (τLVE),
deformation at yield point, YP (γYP), storage and loss moduli at YP (G'G"YP), maximum shear stress
(τmax), and integral z. In general, soil elasticity (γLVE and γYP) and microstructural strength (τLVE and
τmax) were greater in the Oxisols and the Vertisol, which both possess high clay content, while
the latter also contains expansive clay minerals. The lowest structural strength was observed in
the Ultisol which had a high sand content. As rheological properties are related to soil properties
such as particle size distribution and carbon content, they can be applied in the evaluation of
the microstructural strength of clayey and sandy soils and allows for inferences regarding inter-
particle shear strength. However, the test is not applicable to very dry soil samples and sample
preparations can affect the results. We suggest a number of approaches to find solutions for
these difficulties/problems.
Keywords: soil mechanics, oscillatory shear, amplitude sweep test, soil structure

Introduction chemical and mechanical analyses of soils (Baumgarten

et al., 2013). For example, rheometry has been applied to
The processes of deformation and flow of soil the investigation of mineral dispersions and soils (Ghez-
mass originate from microscopic or molecular interac- zehei and Or, 2001; Or and Ghezzehei, 2002; Czibulya et
tions of the constituents (Ghezzehei and Or, 2001). De- al., 2010) and also to studies of the effects of inorganic
formation of soils on the microscale (particle level) due fertilizer and biochar amendment on soil microstructure
to external mechanical stress is related to physicochemi- (Holthusen et al., 2012b, c; Ajayi et al., 2016). Moreover,
cal properties, including particle arrangement and cohe- it has been applied to the study of non-structured soil
sion (Markgraf and Horn, 2009), which in turn depend samples (Markgraf et al., 2006; Baumgarten et al., 2013)
on grain size distribution, shape and type of clay min- and in soils whose natural structure has been preserved
eral, soil organic matter and water contents (Oades and (Holthusen et al., 2012a, b).
Waters, 1991; Markgraf and Horn, 2009; Markgraf et al., These investigations have contributed to the under-
2012), as well as the concentration of salts and cations in standing of the interaction processes on the particle-to-
the soil (Markgraf and Horn, 2009). particle scale, mechanisms for aggregation, strengthening
The more usual physical and mechanical prop- and microstructural stability of different soils, and have
erties measured on the mesoscale are not sufficient to evaluated the effects of water content, texture, mineral-
explain the mechanical processes and forces between ogy, concentration of salts, organic matter content and
soil particles (Markgraf et al., 2006). The theory and ap- soil fertility management on these processes (Markgraf et
plication of soil micromechanics can be better handled al., 2006; Markgraf and Horn, 2007; Pértile et al., 2016).
with rheometry techniques, in which soils are defined However, hitherto, this methodology has rarely been ap-
as viscoelastic materials, since the change in structure plied to subtropical/south Brazilian soils (Markgraf et al.,
involves simultaneous elastic and plastic deformation 2006; Markgraf and Horn, 2007; Pértile et al., 2016), al-
(Mitchell and Soga, 2005; Markgraf and Horn, 2009). though these soils are quite different from the relatively
However, still very little is known about the rheological well investigated European (temperate) soils.
properties of soils. Thus, our aim in this study was to apply the am-
Rheometry is a well-established analysis tech- plitude sweep test, a rheometry technique, to evaluate a
nique applied to various viscoelastic materials (Mezger, number of rheological (micromechanical) properties of
2014), and in the last decade, there have been substan- subtropical soils and highlight the prospects and chal-
tial advances in the use of this methodology for physico- lenges of the methodology viz-a-viz an evaluation of soil

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Pértile et al. Soil rheometry and related difficulties

structural strength. This study is motivated by the grow-

ing application of rheometry to soil research particularly
within temperate regions.

Materials and Methods

Oscillatory shear and amplitude sweep test
Classical mechanics such as Newton’s law of ideal
fluid and Hooke’s law of ideal elastic solids are the basis
for rheometry (Mezger, 2014). However, most materi-
als, like soil, do not behave as ideal systems, since they
exhibit a more complex deformation behavior pattern,
including both elasticity and plasticity (Ghezzehei and
Or, 2001; Schramm, 2006). Under steady stresses, soil
deformation can be described by Bingham's law of vis-
coplastic materials (see also Terzaghi's theory of defor-
mation or precompression stress which maintains that
a soil is stable until a certain critical stress is exceeded
– the “yield stress” according to Bingham).
Based on the different proportions of elastic and
plastic or viscous deformation and flow, rheometry is
applied to the performing of various types of tests, such
as rotation, creep, relaxation, and oscillatory. Oscilla-
tory tests are used to examine all kinds of viscoelastic
materials (Mezger, 2014), including soil (Ghezzehei and
Or, 2001; Holthusen et al., 2010). The principles of this
test can be explained with the help of a parallel plates
model: a sample is placed between two plates, the low- Figure 1 – Model of parallel plates in oscillatory shear tests (s =
er plate being fixed while the upper plate is rotated deflection distance, φ = angle of deflection; h = distance between
in an oscillatory manner (Figure 1) (Mezger, 2014), i.e. plates) (A); and schematic results of an amplitude sweep test with
the plate is shifted alternately to the right and the left, increasing deformation (γ) and shear stress (τ) as a function of
in a sinusoidal function of time with at first a small time (t) (B). For viscoelastic substances, such as soil, the phase
deflection angle (φ, °), creating a laminar flow within shift angle (δ) of τ from γ is between 0 and 90°. Source: adapted
theoretically infinitesimal thin layers (Schramm, 2006). from Mezger (2014).
Thus, the deflection of the upper plate follows a similar
sinusoidal function, while the deflection of the lower
plate is zero (s = 0), generating resistance stresses or ior (Markgraf et al., 2006). During an amplitude sweep
deformations in the sample (Schramm, 2006; Holthu- test, the deformation amplitude increases over time, for
sen et al., 2010). example, between 0.0001 % and 100 % (Holthusen et al.,
In oscillatory tests, γ is calculated as the ratio of 2010). Deformation of 100 % occurs when deflection is
the deflection distance (s, m) and the distance between equal to distance between the plates (s = h) and, conse-
the plates (h, m) (Eq. 1). In the case of parallel circular quently, the deflection angle φ equals 45°.
plates, as is commonly used, s is determined as the de- The relationship between controlled γ and result-
flection at the outermost edge of the plate (Figure 1A). ing τ is further described by the phase shift angle (δ, °)
The shear stress (τ, Pa) results from the force required as characteristics of the soil (material) (Holthusen et al.,
to generate a deformation (γ, %) along the shear surface 2010). Perfectly elastic substances react directly on the
(Holthusen et al., 2010). deformation, and therefore, τ and γ curves are in phase,
with δ = 0°, while conversely, δ = 90° is characteristic
s
γ = 100 (1) of a perfect fluid. For viscoelastic substances, hence, τ
h
shows a temporal lag with respect to γ of the type 0 < δ
The amplitude sweep test, among the oscillatory < 90° (Figure 1B) (Mezger, 2014).
tests, has been the most widely used in soil investiga-
tions, being characterized by a variable amplitude (of de- Determination of rheological properties
formation or shear stress) at a constant frequency (Mark- To quantify rheological properties of viscoelastic
graf et al., 2006). Either τ is defined and the resulting γ materials by oscillatory shear tests, certain parameters
is measured or vice versa (Markgraf et al., 2006). The have been adapted from classic mechanics. While, accord-
latter, called “controlled shear deformation – CSD” has ing to Hooke's law, the shear modulus (G) under uniaxial
generally been used to assess microstructural soil behav- stress conditions is constant for perfectly elastic substanc-

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Pértile et al. Soil rheometry and related difficulties

es (Mezger, 2014); for oscillatory stresses a complex shear

modulus (G*, Pa) is adapted (Eq. 2), which is divided into
a storage modulus (G', Pa) (Eq. 3) and a loss modulus (G",
Pa) (Eq. 4) (Holthusen et al., 2010; Mezger, 2014).

G* = τA /γA (2)
τ
G′ = G ∗cos δ = A cos δ (3)
γA
τ
G′′ = G sin δ = A sin δ
∗
(4)
γA
where τA is the amplitude of τ (Pa) and γA is the ampli-
tude of γ (%).
The storage modulus G' represents the elastic
component of a material, indicating that part of the
induced energy by the external stress is temporarily
stored during the test to be retrieved upon the removal
of stress. The loss modulus G" is the viscous component
or imaginary lost energy, which means that the energy
used to initiate the flow is irreversibly lost (Markgraf et
al., 2006; Schramm, 2006; Mezger, 2014). Both moduli
G' and G", depend directly on γ, τ and δ (Holthusen et
al., 2010) recorded during the test.
The ratio of G" and G' results in tan δ (dimension-
less) (Eq. 5), also referred to as loss factor, since it indi- Figure 2 – Schematic results of an amplitude sweep test: storage
cates the fraction of energy which is lost upon defor- modulus (G’), loss modulus (G”) and loss factor (tan δ) as a function
mation (Horn and Peth, 2011). When tan δ < 1 (G' > of deformation (γ), plotted on a logarithmic scale (A); and shear
G"), the elastic component predominates; and when tan stress (τ) as a function of deformation (γ) (B). Source: Pértile et
δ > 1 (G' < G"), the viscous component is predominant al., 2016.
(Markgraf et al., 2006). Thus, similar to δ, tan δ can be
used to classify the mechanical strength of soil samples The integral z and the maximum shear stress (τmax,
(Holthusen et al., 2010; Baumgarten et al., 2013). Pa) have also been applied as rheological properties. The
integral z (dimensionless) is calculated as the area lim-
G ′′
tan δ = (5) ited on the one hand by the curve of tan δ, from the
G′ lowest applied deformation (here γ = 0.0001 %) to the
For the curves of G' and G" as a function of γ (on a crossover, where tan δ = 1, and on the other hand the
logarithmic scale), a linear viscoelastic range (LVE range) line of tan δ = 1 itself (Figure 2A). The greater the inte-
is determined, namely via the end of the LVE range at gral z value, the higher the overall proportion of elastic
the limit of deformation (γLVE, equal to γL in some publi- deformation (as represented by G’), and therefore, the
cations, %) (Figure 2A) (Markgraf et al., 2006; Holthusen higher the rigidity of the soil (Markgraf et al., 2011). Ad-
et al., 2010). The LVE range is defined as the range of de- ditionally, τmax is the maximum τ shown by the sample
formation where G*, consisting of G' and G", is constant during the amplitude sweep test (Figure 2B), indicating
(Schramm, 2006); i.e. as long as the γLVE is not exceeded the maximum shear strength of a sample (Holthusen et
no significant change in the soil internal structure oc- al., 2012a). Further shear stress values used are τ cor-
curs and deformation is reversible, while deformation responding to γLVE and γYP, respectively, τLVE, Pa (equal to
beyond γLVE causes irreversible changes in the sample, yield stress τy in some publications) and τYP, Pa (equal to
which is indicated by a decrease in G' and G" (Holthu- flow stress τf (Mezger, 2014)).
sen et al., 2010; Mezger, 2014). The τ values are calculated from the recorded
From the curves of G' and G" versus γ also their torque (M, Nm) necessary for the controlled deforma-
point of intersection (crossover or yield point - YP) is ob- tion, and the plate radius (r, m) (Eq. 6) (Mezger, 2014).
tained where tan δ = 1 and G' = G" (G'G"YP, Pa); i.e. the
elastic and viscous components are equal (Figure 2A) 2M (6)
τ=
(Holthusen et al., 2010). This point occurs already in the πr 3
non-linear deformation range (Mezger, 2014) and is the
critical deformation (γYP, %) in which the viscous com- This set of rheological properties (γLVE, τLVE, γYP,
ponent exceeds the elastic and the sample flows, irre- G'G"YP, τmax and integral z) provides key information
versibly modifying the particle arrangement (Markgraf about microstructural soil resistance (Markgraf et al.,
et al., 2006; Schramm, 2006; Mezger, 2014). 2011).

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Pértile et al. Soil rheometry and related difficulties

Table 1 – Description and characterization of the examined soils of Rio Grande do Sul, Brazil.
Soila Symbol Geographic coordinates Altitude Sand Silt Clay TC CEC ρB
m ----------------------- g kg–1 ----------------------- cmolc kg−1 kg m–3
Rhodic Kandiudox Oxisol 1 28°38'17.83" S; 53°5'6.91" W 412 160 236 603 23.2 5.9 0.91
Typic Hapludox Oxisol 2 28°30'38.09" S; 50°52'46.15" W 967 84 400 516 33.6 11.8 1.10
Arenic Hapludult Ultisol 30°41'25.23" S; 55°7'50.11" W 165 844 98 57 6.2 2.2 1.66
Oxyaquic Hapluderts Vertisol 30°43'9.00" S; 55°47'38.56" W 233 87 476 437 44.1 43.0 0.94
a
Classification according to Soil Taxonomy (USDA, 2010); Sand, silt and clay = determined according to Suzuki et al. (2015), with sodium hydroxide (Oxisols and
Ultisol) and sodium hexametaphosphate (Vertisol) dispersant solution (Donagema et al., 2011); TC = total carbon, determined by dry combustion of soil macerated
at autoanalyzer; CEC = cation exchange capacity, determined according to Donagema et al. (2011); ρB = bulk density, determined according to Blake and Hartge
(1986) in samples obtained with preserved structure.

Figure 3 – Rheometer and measuring system of parallel plates (A). Soil sample preparation, consisting of: a horizontal cut (B), and a vertical cut
(C); sample ready for the test after removal of excessive soil (D) and sample perfectly adjusted to the gap, i.e. the space between the plates (E).

Soil analysis rheometer (MCR 102, Anton Paar, Germany) equipped

In order to conduct amplitude sweep tests, soil with parallel plates: a fixed lower plate of 50 mm in
samples were collected from the superficial horizon of diameter and an upper rotating plate of 25 mm in di-
four soil classes of the state of Rio Grande do Sul (RS), ameter, both roughened (Figures 3A, D) to optimize
southern Brazil (Table 1). These samples were collected contact of soil and plate (MCR 102, PP25/P2 model,
from native forest - Rhodic Kandiudox (Oxisol 1), culti- Anton Paar, Germany). From the repacked samples, a
vated pasture - Typic Hapludox (Oxisol 2), and natural volume of approximately 4 cm³ was used in the rheom-
pasture - Arenic Hapludult (Ultisol) and Oxyaquic Hap- etry tests. To ensure minimal disturbance, the samples
luderts (Vertisol). were placed on the lower plate of the rheometer and
The soil samples collected were air-dried and gently pushed out of the rings. The samples were cut
sieved through a 2 mm mesh. In all the soil types, mi- to a height of about 4.5 mm with nylon yarn and/or
cro-aggregates were found, but those from Oxisol 2 and stiletto (Figure 3B) and vertically cut to size with a bev-
Vertisol were the most stable. The air-dried fine soil eled ring of 25 mm diameter (Figure 3C) immediately
fraction (< 2 mm) was slightly moistened and stored before the test. The test samples were treated so as to
hermetically sealed for approximately 16 h. The wet exactly fit the diameter of the top plate and the gap
soil was then transferred to rings (3.6 cm diameter (sample height) (Figures 3D, E), to avoid any possible
and 1.0 cm height) and slightly compacted to a density effects of the surrounding soil (Holthusen et al., 2010)
equal to the average value of the soil bulk density (ρB) and ensure the equality of the initial conditions for all
in the field (Table 1). The samples (three samples by samples. To prevent loss of moisture, it was important
soil) were then saturated by capillarity rise with dis- that the samples were prepared as promptly as possible
tilled water and subsequently drained to -3 kPa on sand prior to measurement.
columns (Reinert and Reichert, 2006). The amplitude sweep tests were performed un-
Amplitude sweep tests at constant frequency and der the following conditions: constant temperature
temperature were performed with a modular compact of the lower parallel plate = 20 °C (controlled by a

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Pértile et al. Soil rheometry and related difficulties

Peltier unit); gap = 4 mm (Figure 3E); resting period content loss of more than 10 % were excluded due to
before the test = 30 s; variation of amplitude of de- the strong impact of water content on soil mechanics/
formation = 0.0001 to 100 %; angular frequency = rheology.
0.5 Hz; and number of measuring points = 30 (ac-
cording to Markgraf et al., 2006). Test duration was Results and Discussion
about 14 min, which ensured minimal water loss
from the sample during the test. The normal force Rheological properties
on the sample did not exceed 12 N at the beginning Soil rheological behavior was assessed from the
of the test (Markgraf et al., 2006) (to obtain adequate curves of G' and G" as a function of γ (both in logarith-
sample-to-plate contact) and tended to 0 N in the end mic scale) (Figure 4) and according to the properties
of the test. derived from the amplitude sweep test results (Table
Using the Rheoplus/32 V3.62 software program 2). In the following discussion, we will follow an order
(Anton Paar, Germany) the rheological properties as in which the properties “appear” during the amplitude
described in the previous chapter were derived. The sweep test, starting with the initial values of G' and G".
first three points of the 30 measuring points were ex- With increasing deformation, the nature of the proper-
cluded because of the lower sensitivity of the rheom- ties is changing: While the LVE range properties are
eter used (e.g. compared to a MCR 302, Anton Paar, useful for describing “purely” elastic behavior (or fully
Germany), when φ < 1 μrad. Samples with a water recoverable deformation), the maximum shear strength

Table 2 – Mean values and standard deviation of rheological properties and gravimetric moisture (θg) of soils (N = 3) at matric potential of -3 kPa.
Soil γLVE τLVE γYP G'G"YP τmax Integral z θg
% Pa % ---------------------------------------- Pa ---------------------------------------- - g g−1
Oxisol 1 0.009 (± 0.001) 116 (± 12) -a -a 1082 (± 146) 62 (± 4) 0.45 (± 0.01)
Oxisol 2 0.039 (± 0.001) 457 (± 103) 72 (± 5) 501 (± 423) 2702 (± 718) 34 (± 6) 0.51 (± 0.00)
Ultisol 0.005 (± 0.000) 93 (± 43) 56 (± 7) 666 (± 23) 698 (± 264) 22 (± 2) 0.24 (± 0.02)
Vertisol 0.045 (± 0.001) 171 (± 12) 62 (± 4) 656 (± 109) 1094 (± 73) 24 (± 2) 0.78 (± 0.01)
γLVE = deformation at the end of the linear viscoelastic range (LVE range); τLVE = shear stress at the end of LVE range; γYP = deformation at yield point (YP); G'G"YP =
storage and loss moduli at YP; τmax = maximum shear stress; aNo crossover detected.

Figure 4 – Storage and loss modulus (respectivelly, G’ and G”) and loss factor (tan δ) versus deformation (γ), on a logarithmic scale (pairs of lines
correspond to repetitions), of soils at a matric potential of -3 kPa.

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Pértile et al. Soil rheometry and related difficulties

is independent of the concepts of elasticity or plasticity one hand, high clay and TC content in the Vertisol (Table
and denotes the shear resistance of the soil. The yield 1) increased the elasticity due to adsorbed water, includ-
point is based upon the transition from mostly elastic ing (basic) cations in the soil solution and on the surfaces
(G' > G") to mostly plastic behavior (G" > G'). In cer- of the expansive clay mineral (smectite) (Markgraf et al.,
tain soils (as the Oxisol 1, see Table 2 and Figure 4), this 2006). On the other hand, soils with higher kaolinite con-
transition is not achieved within the chosen range of tent and of coarse texture are less elastic (i.e. γLVE is lower)
the amplitude sweep test (0.0001 to 100 % of deforma- (Markgraf and Horn, 2007), as is especially the case for
tion) (cf. Markgraf et al., 2011; Baumgarten et al., 2012; the Oxisol 1 and the Ultisol (Tables 1 and 2). While in
Pértile et al., 2016). As a consequence of their different the Ultisol sandy texture and poor aggregation are sup-
characteristics and determination, the different rheo- posedly the reason for the overall low stability and elas-
logical properties can indicate different directions of ticity, in the Oxisols the existence of pseudosand seems
microstructural strength (stabilization vs. destabiliza- to play a fundamental role. Both Oxisols exhibit pseu-
tion) within the same soil. dosand - stable microaggregates of sand diameter, but
The initial values of G' and G" differed between those in the Oxisol 2 are larger and more stable due to
soils. For both Oxisols, the G' and G" values were, re- a higher abundance of goethite (yellow-brownish color),
spectively, ≈ 106 and ≈ 105 Pa (Figure 4). For the Ultisol while the Oxisol 1 is dominated by hematite (red color)
these values were slightly higher, and for the Vertisol (data not shown). Only in the Oxisol 1, did the aggrega-
slightly lower, which is in agreement with the results of tion due to oxides (pseudosand) present a high degree of
Markgraf et al. (2006). Higher values of G' and G" indi- similarity with the sandy Ultisol (regarding LVE range
cate higher rigidity, which is related to the influence of properties), while the stronger, more concentrated ag-
texture, soil organic matter (SOM) and clay mineralogy gregated Oxisol 2 showed a broader LVE range and the
(Markgraf and Horn, 2007), i.e. clay soils show higher highest corresponding shear resistance.
structural rigidity than silty substrates (Markgraf and Further to the LVE range, the Ultisol exhibited an
Horn, 2006a), as well as soils with higher contents of Fe apparent increase in G" (Figure 4), i.e. there was a rela-
oxides and SOM (Markgraf and Horn, 2007), since these tive increase in plasticity. The tan δ curve, including sim-
factors promote favorable mechanisms for soil aggrega- ilar information about the deformation behavior during
tion (Baumgarten and Horn, 2013). the oscillatory shear, also showed a more pronounced
The Ultisol was expected to exhibit the lowest val- increase in tan δ between γ of 0.01 and 10 %, followed
ues for G' and G" as it has the lowest content of clay, by a decrease in the Oxisol 1 and the Ultisol (Figure 4).
organic matter and basic cations and is thus poorly ag- In both cases, this behavior is due to the reorientation
gregated. Therefore, it can be assumed that the high of soil particles such as kaolinite platelets, individual
density of this soil increases its stability, especially as packages or grains (Markgraf and Horn, 2007), which
further properties denote low rigidity. The higher the was not observed in the Vertisol and was less expres-
density of a soil, the higher its shearing resistance and sive in Oxisol 2, both with higher clay contents (Table
the lower the compressibility (Horn and Peth, 2011). 1). After the particles align, elasticity (G') is increased
The relatively higher initial values of G' and G" for the relative to plasticity (G") again (Markgraf et al., 2006).
Oxisols compared to the Vertisol are in accordance with This behavior was observed in the Oxisol 1, clayey and
the findings of Markgraf and Horn (2007) for samples aggregated, possibly due to low ρB and presence of pseu-
drained to -6 kPa. Markgraf and Horn (2006b) also mea- dosand, and in the Ultisol due to high sand content (Ta-
sured higher initial values of G' and G" due to low γ, i.e. ble 1), which might cause dilatancy, i.e. an increase in
the higher the G' and G", the more stable the soil ini- shear resistance due to friction and restricted rotation of
tially. However, there is not necessarily a direct relation- the sand and sand-like aggregates. Similarly, Markgraf
ship with the properties of the LVE range. It is assumed et al. (2006, 2011) and Markgraf and Horn (2006a, 2007)
that the wider the LVE range (greater γLVE), the higher observed this behavior in sandy and silty substrates, ka-
the elasticity of the soil, i.e. the recoverable deforma- olinitic clay soils and soils with presence of pseudosand
tion (Markgraf et al., 2006). The LVE range was smaller due to extreme shear strength (larger angle of internal
for the Oxisol 1 and the Ultisol than for the Oxisol 2 friction).
and the Vertisol (Figure 4, Table 2). The higher values The yield point, which indicates the transition
of γLVE in the Vertisol probably derive from higher total from (mainly) elastic to (mainly) viscous deformation,
carbon content (TC) as well as from high clay content and occurred at relatively high deformations γYP (Figure 4).
the presence of smectite. Carbon acts as a strong bind- The largest values for γYP were observed in the Oxisol 1
ing agent increasing soil stability (Six et al., 2004; Bronick (>100 %, no yield point, i.e. very high stability, no gel-
and Lal, 2005; Kögel-Knabner et al., 2008; Holthusen et character is reached), followed by the Oxisol 2 (72 %),
al., 2012a). This effect was confirmed by a decrease in the Vertisol (62 %), and the Ultisol (56 %) (Table 2).
γLVE in soils subjected to oxidation of SOM to determine This result seems related to higher Fe oxides content of
the stabilizing effect of SOM (Markgraf and Horn, 2007). Oxisols 1 and 2 (data not shown), which are strong ce-
Markgraf and Horn (2007), furthermore, observed a high- menting agents (Six et al., 2004; Bronick and Lal, 2005).
er γLVE in a Vertisol compared to different Oxisols. On the Although we also expected a greater influence of TC

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Pértile et al. Soil rheometry and related difficulties

content on γYP (Baumgarten et al., 2013), this was not Furthermore, in direct comparison with the Oxi-
seen clearly. Soils with higher cation exchange capacity, sols, the different results for the different rheological
soil carbon and Ca2+ content can be deformed to a great- properties indicate diverse types of aggregation and/or
er extent before flow, i.e. possess a higher γYP (Markgraf bonds between particles: the Oxisol 1 showed elasticity
et al., 2011), but according to Markgraf and Horn (2007) over a large range of deformations by means of integral
Fe oxides have a more stabilizing effect on the micro- z, but for others properties behave like a sandy soil de-
structural stability than, for example, the TC content. spite a very high clay content of 603 g kg−1, due to the
In addition to the Fe oxides, the γYP is influenced presence of microaggregates (pseudosand). It is possible
by soil texture. For the Ultisol with loamy sand texture that lower stability of these microaggregates enabled
and low water content at -3 kPa (Table 2), the γYP was the particles to rearrange at higher deformation levels
lower than for the more clayey Oxisol 2, and the Verti- in stable arrangements of high friction. The Oxisol 2, on
sol (Table 1), which had higher elasticity. Markgraf and the other hand, with continuous increases in microag-
Horn (2006a) also observed lower γYP in a sandy loam gregate stability compared to the Oxisol 1 (as proven by
Haplic Chernozem compared to a silty loam Luvisol. haptic test), had the highest friction and cohesion (as
The Oxisol 1 did not exhibit a yield point, which, as seen by shear stress properties τLVE and τmax), though the
stated earlier, is indicative of a high degree of micro- bonds were lacking in elasticity, i.e. once they are de-
structural stability (Markgraf et al., 2011; Baumgarten stroyed, the soil does not regain its structure under the
et al., 2012). Markgraf and Horn (2007) also did not ob- impact of transient stresses as it does during an ampli-
serve a yield point in clay-rich Oxisols, indicative of the tude sweep test (little thixotropy).
very rigid character of these soils, as noted in the Oxisol Thus, the results of the amplitude sweep test con-
1 even with lower bulk density (less number of contact firm previous research (Markgraf et al., 2006; Markgraf
points between particles) than in the other soils (Table and Horn, 2007; Markgraf et al., 2011; Holthusen et al.,
1). Despite the low bulk density, the soil strength can be 2012a, c; Baumgarten et al., 2013; Pértile et al., 2016) in
high due to an extremely stable arrangement of the soil proving that rheological properties are influenced by soil
particles and the cementation between particles (Dexter, texture, mineralogy and carbon content.
1988; Horn and Dexter, 1989) by clay minerals, oxides
and inorganic and organic compounds (Dexter, 1988). Difficulties and opportunities
Integral z was lower for Oxisol 2, Ultisol and Verti- In general, rheological properties are obtained
sol, and highest for the Oxisol 1 (Table 2). The high inte- from materials/dispersions with a high water content. If
gral z value, thus, confirms the greater structural rigidity the soil water content is low, the sample cannot deform
of the Oxisol 1. Although the shear stress properties and homogeneously, which decreases the accuracy of rheo-
the LVE range do not suggest a very elastic and stable logical properties (Mezger, 2014). Therefore, samples are
microstructure of this soil, our results are supported by commonly drained up to - 1 to -6 kPa. In some cases, -15
Baumgarten et al. (2013), who also found similar values kPa was applied (Markgraf et al., 2011). Consequently,
for sandy to loamy soils developed from volcanic ash, the use of rheological properties to predict soil deforma-
while silty to clayey soils had integral z values of 30 to tion in the field is limited to the moisture range from
50 at -6 kPa. Furthermore, the Vertisol has quite a high saturation to around -6 or -10 kPa. In the field, most soil
water content, and sheared during the amplitude sweep tillage and crop management practices are carried out
test possibly causing liquefaction, intensified by sup- when the soil water content is lower (below field capac-
posedly low conductivity (water pressure cannot regain ity) than that used in rheometry. Thus, soil deformation
equilibrium so fast), while in the other soils both the caused by machinery traffic with low water content in
conductivity is higher and the water content lower. the soil may not be fully explained by the rheological
The τLVE, τmax and G'G"YP are also useful properties properties, since as long as the dynamic forces are rela-
for the rheological characterization of the soils. The τLVE tively small, the static stress strain processes may domi-
and τmax were lowest for the Ultisol (Table 2), the sandi- nate the whole procedure. However, rheometry can be
est soil (Table 1) and G'G"YP was similar between soils, very important in situations such as landslides on slopes
considering the high standard deviation values. The τmax where low magnitude stresses cause devastating events
indicates the maximum soil shear strength (Holthusen during rainstorms (Horn and Peth, 2011).
et al., 2012b), which was greater for the clayey soils in Moreover, the soil structure was not preserved in
this study. Soil shear strength may also increase with our samples and nor were those of other investigations
increasing ρB (Holthusen et al., 2012a), but for our soils, prepared for rheometry. To overcome this particular
τmax and τLVE increased with clay content even with very problem, recent studies are using samples with pre-
low ρB values (especially, Oxisol 1 and Vertisol) (Table 1). served structures (Holthusen et al., 2012a, b), which
Thus, the Oxisol 2, clayey and with comparatively high- would provide the most representative rheological
est bulk density (1.10 kg m−3, Table 1) had the highest properties of the microstructure resistance of field soil.
τLVE and τmax. Therefore, soil composition appears to be However, a further problem has to be solved: in sam-
more important than bulk density for shear strength of ples with preserved structures, the spatial distribution
the soil, in agreement with Czibulya et al. (2010). of particles and microaggregates is not homogeneous,

Sci. Agric. v.75, n.2, p.154-162, March/April 2018 160

Pértile et al. Soil rheometry and related difficulties

and plant root can be present. These factors might pro- Conclusions
mote heterogeneous soil deformation during amplitude
sweep tests and increase the variation in rheological In general, as interpreted from our results, an
properties between repetitions in the same soil. In ad- increase in rheological properties represents increased
dition, changes in density is likely to affect rheological soil microstructure resistance, but these rheological
behavior patterns. Thus, further studies are needed to properties seem to be affected by different soil proper-
validate the use of samples with preserved structures ties. Soil microstructural strength was greater in soils
(and those of different density due to structural distri- with higher clay and oxides content, and elasticity was
bution). greater in soils with higher clay content and expansive
Moreover, rheometry studies generally use ho- clay, while sandy soil (both naturally and by aggrega-
mogeneous soil samples and establish the same ρB tion, “ecologically sandy”) showed lower elasticity and
value for different soils, which is an advantage due to sandy soil (naturally) showed lower structural strength.
reducing independent variables which influence the However, these relations have been little investigated;
rheological properties. However, the ρB varies with thus, it should be further elucidated which soil physi-
soil composition, genesis and management (factors cal and chemical properties influence each rheological
considered in preparing the samples of this study) property and in what way.
and, in this case, the preparation of samples with the Thus, the amplitude sweep test (rheometry) for
same ρB does not represent the density condition in mechanical evaluation in the soil particle scale and
the field. Thus, studies are needed to determine the microaggregates is a modern technique that is already
influence of ρB on the rheological properties of differ- well established. However, this test is restricted to high
ent soils. matric potentials (i.e. saturation to approximate field
In the amplitude sweep tests, there is also great capacity), hindering its application for the evaluation
influence of normal stress (σ) on rheological proper- of soil deformation caused by machinery in ideal traffic
ties (Buchmann et al., 2015). We observed responsive conditions (low water content). Furthermore, we must
increases in initial moduli G' and G" caused by an in- be attentive to factors that affect the rheological prop-
crease of the σ, as annotated by an increase in the initial erties such as the soil density of the prepared samples,
normal stress (σi); (because the MCR 102 rheometer is the use of undisturbed soil samples, and normal stress
not able to record the σ during testing, the σi is manually before and/or during the test. For a better understand-
annotated). In the amplitude sweep test, the gap is kept ing of these factors, we suggest additional studies with
constant, but the σi cannot be fixed, it is only kept at less undisturbed soil samples and homogenized soil samples
than 12 N (Markgraf et al., 2006) with the sample prepa- of different densities. Further work is also required on
ration. Even with the careful preparation of samples it is the use of rheometry as a tool for the assessment of soil
difficult to maintain the same value of σi in all tests, be- deformation under conditions of high soil water con-
cause σi varies with particle size, density, water content tent, such as in areas prone to erosion and landslide.
of the soil, and small variations in sample height. How-
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