Article

Permeability Coefficient of Low Permeable Soils

as a Single-Variable Function of Soil Parameter
Tomasz Kozlowski * and Agata Ludynia
Faculty of Environmental, Geomatic and Energy Engineering, Kielce University of Technology,
25-314 Kielce, Poland; [email protected]
* Correspondence: [email protected]

Received: 16 September 2019; Accepted: 22 November 2019; Published: 27 November 2019

Abstract: Based on the results of experimental studies concerning the filtration coefficient, the
Darcianity of the observed flows for eight cohesive soils at four hydraulic gradients was analyzed.
It is observed that linear dependence of flow velocity on hydraulic gradient is an approximation
only, and it is the worse the more cohesive a given soil is. Despite this, Darcy’s law can be a correct
approximation of the empirical relationship between hydraulic gradient and the flow velocity, also
in very cohesive soils. A statistical analysis was carried out to identify correlation between soil
properties and permeability coefficient. For each soil, 109 parameters were analyzed, among others
applying mercury intrusion porosimetry, scanning electron microscopy, dynamic image analysis,
and laser diffraction. Ultimately, three single-variable models best fitted to the experimental data
were found, using the plasticity index IP as the independent variable, the average pore diameter DP,
and the convexity of silt fraction particles. All model parameters are statistically significant at p <
0.05. Comparison with reference multi-variable models showed that the best fit for experimental
data is observed by the model with the plasticity index, while the results suggest low usability of
single-variable models with structural parameters.

Keywords: permeability coefficient; cohesive soils; Darcianity of flow; plasticity index; convexity of
particles; void ratio; pore diameter

1. Introduction
Increasing interest in cohesive soils and clay minerals has been observed in recent years on the
part of environmental engineering. Soils of this type show a tendency for particles to stick to each
other due to intermolecular interactions and, as a result, they usually have low permeability. This is
due to the properties of these materials, allowing use of them, among others, as pollution sorbents
and mineral insulating barriers at landfills, including those used for radioactive waste. Any soil
which is to be used as a barrier needs to have low permeability, self-sealing capability, and high
cation exchange capacity [1,2]; hence, thorough examination of the mentioned parameters is crucial.
Insufficient or even incorrect testing of soils in this regard may result in underground water
contamination with various substances coming from municipal and industrial wastes stored in
landfills. For example, in the case of industrial waste storage (acidic waste water), underground water
protection is implemented using clay minerals, which are required in order to reduce hydraulic
conductivity of clays occurring naturally beneath landfills [1]. Cohesive soils and clay minerals are
also used in urban solid waste storage facilities and mine waste dumps as barriers and sealings [3].
They also work as geological reservoirs used to store carbon dioxide [4]. At the same time, bentonites
are used to store radioactive and other hazardous waste because they have proved to have special
expansive properties and high water adsorption potential [3,5–7]. Moreover, they are used to
eliminate toxic chemical compounds from environment when reducing the extent of pollution

Water 2019, 11, 2500; doi:10.3390/w11122500 www.mdpi.com/journal/water

Water 2019, 11, 2500 2 of 21

dispersion in soil, water, and air [6,8]. Bentonites are also used in the production of impermeable
geosynthetic mats and geomembranes resistant to aggressive chemical agents [9].
Erroneous analysis of factors determining soil permeability may involve serious consequences
because a disadvantageous effect of filtration is manifested by the loss of soil medium stability. These
phenomena may include: suffusion (washing of mineral particles), quicksand (soil liquefaction),
hydraulic penetration, or replacement. Negative impact of the filtration forces on soil is observed, for
example, in the vicinity of flood banks when water level is high in rivers (most often at the foot of
landside slope and drainage facilities), and while making constructional foundation trenches (there
is the risk involving the loss of soil stability in riverbed and slopes). These areas of disturbed balance
due to water migration and their further uncontrolled growth may be the reason for various
breakdowns [10]. Stringent requirements resulting from the need to protect environment entail
greater interest in adequate evaluation of geotechnical parameters, including permeability coefficient
[11]. Regarding mentioned environmental engineering problems, it is extremely important to know
geotechnical parameters and mechanisms determining soil permeability [12–14].
However, while one can find many empirical equations useful in estimating the value of
permeability coefficient for coarse soils or sediments (sands and gravels), solutions applicable to
poorly permeable soils are significantly rarer. Some of these “coarse” formulas are attempted to be
used in cohesive soils (especially the so called Kozeny-Carman formula introduced in first half of
20th century [15]), but, as not taking into account the water-mineral interactions manifesting as the
soil plasticity, all of them seem less useful in such a context. There are presented a number of
empirical formulas used to calculate the permeability coefficient for different soil types on the basis
of their selected parameters [16–20]. However, these empirical or semi-empirical models were
introduced without any statistical treatment, and it is not clear how high absolute and relative mean
errors can be expected and if the estimates of model parameters are statistically significant. In other
words, it is hard to assess their predictive capacity in terms of modern statistics.
This study presents an attempt to find empirical single-variable models on the basis of the results
of owned permeability coefficient measurements on samples of eight poorly permeable soils, which
differ considerably in their mineralogical composition, origin, and physical and structural properties.
The search for the models was carried out without making any presumptions regarding lesser or
greater usability of a given parameter, meaning that all 109 analyzed parameters constituted
equivalent input data. Soil parameters were divided into two groups: physical parameters and
structural parameters, the latter requiring more refined experimental techniques, such as mercury
intrusion porosimetry (MIP), scanning electron microscopy (SEM), dynamic image analysis (DIA),
and laser diffraction method (LD). According to the initial hypothesis, models based on structural
parameters may prove to be more perfect, although physical parameters, such as the plasticity index
and the Atterberg limits, may include more information on the clay-water interaction and are more
easily accessible as no specialized equipment needs to be used to determine them.
However, an attempt to search for models with the number of soil parameter limited to one has
an essential theoretical meaning, allowing for a strict identification of soil properties most responsible
for the flow phenomena in clay-water systems.

2. Materials and Methods

2.1. Materials
Eight cohesive soils were subject to experiments, numbered from 1 to 8 for the identification
purposes. The soils were collected in Poland in the region of Swietokrzyskie Mountains. Pursuant to
Polish standard [21]/European standard [22], they were named as follows: soil 1—loamy sand/silty
sand-siSa, soil 2—sandy clay/silty sand-clSa, soil 3—clay/clay-Cl, soil 4—loam/silty clay-saclSi, soil
5—clay/clay-Cl, soil 6—firm silty clay/clay loam-sasiCl, soil 7—clay/clay-Cl-siSa, and soil 8—
silt/sandy silt-saSi. Basic characteristics of the soils are presented in Table 1, while selected structural
properties are given in Table 2.
Water 2019, 11, 2500 3 of 21

Table 1. Basic properties of studied soils.

Parameter Method Soil 1 Soil 2 Soil 3 Soil 4 Soil 5 Soil 6 Soil 7 Soil 8
Bulk density ρ, (t/m3) ring 2.09 2.08 1.97 2.11 1.89 2.06 2.17 2.04
Dry density ρd, (t/m3) calculations 1.74 1.67 1.40 1.85 1.37 1.54 1.39 1.73
Specific gravity Gs pycnometer 2.59 2.62 2.56 2.66 2.54 2.68 2.67 2.67
Porosity ncalc, (-) calculations 0.33 0.36 0.45 0.31 0.46 0.43 0.48 0.35
Void ratio ecalc, (-) calculations 0.49 0.57 0.83 0.44 0.85 0.74 0.92 0.54
Saturated void ratio esat,
calculations 1.84 3.07 4.12 2.91 4.24 3.96 3.84 1.85
(-)
Water content, (%) dryer-balance 19.8 25.0 40.8 14.2 37.5 33.5 56.0 18.0
Saturated water content
dryer-balance 129 224 294 209 290 280 294 118
wsat, (%)
Plastic limit wP, (%) rolling 13.50 14.04 19.78 10.27 34.80 15.27 15.50 15.39
Liquid limit wL, (%) Casagrande 21.87 29.30 64.21 26.37 62.55 35.82 71.34 20.22
Plasticity index IP, (%) calculation 8.4 15.3 44.4 16.1 27.8 20.6 55.8 4.8
Colloidal activity, (-) calculations 0.93 1.09 1.23 1.24 0.51 0.89 1.36 0.69
Organic matter content,
roasting 1.39 1.99 4.45 2.31 0.00 4.29 2.74 1.7
(%)
Content of fraction
hydrometric 9.00 14.00 36.00 13.00 54.00 23.00 41.00 7.00
fi < 2 μm, (%)
Content of fraction
hydrometric 27.00 28.00 48.00 46.00 46.00 52.50 48.00 66.00
2 < fπ < 50 μm, (%)
Content of fraction
hydrometric 62.00 57.80 16.00 39.50 0.00 24.00 11.00 26.00
50 < fp < 2000 μm, (%)
Content of fraction
laser diffraction 6.71 6.38 15.19 10.01 25.51 17.06 26.29 5.79
fi < 2 μm, (%)
Content of fraction
laser diffraction 24.48 33.10 57.06 37.68 74.47 46.70 55.98 70.97
2 < fπ < 50 μm, (%)
Content of fraction
laser diffraction 67.07 60.06 27.76 50.35 0.02 35.77 17.61 23.24
50 < fp < 2000 μm, (%)

Table 2. Structural properties of studied soils.

Parameter Method Soil 1 Soil 2 Soil 3 Soil 4 Soil 5 Soil 6 Soil 7 Soil 8
Void ratio, (-) MIP 0.341 0.265 0.224 0.367 0.749 0.156 0.142 0.591
Porosity, (-) MIP 0.254 0.210 0.183 0.268 0.428 0.135 0.124 0.372
Content of pores P < 3 nm, (%) MIP 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00
Content of pores 3 < P < 10 nm, (%) MIP 4.66 2.13 12.08 4.71 1.11 41.75 41.04 0.38
Content of pores P > 10 nm, (%) MIP 95.34 97.87 87.92 95.29 98.89 58.25 58.96 99.62
Volume of intrusions V, (mL/g) MIP 0.13 0.10 0.08 0.14 0.29 0.06 0.05 0.22
Mean pore diameter D, (nm) MIP 137 125 41.4 113 69.6 15 14.8 404
Sphericity of particles, (-) DIA 0.859 0.852 0.87 0.858 0.809 0.837 0.854 0.862
Aspect ratio of particles, (-) DIA 0.715 0.697 0.702 0.7 0.647 0.689 0.723 0.683
Convexity of particles, (-) DIA 0.893 0.894 0.866 0.898 0.851 0.891 0.901 0.88.
Specific surface area for fraction fi < 2 μm,
LD 0.410 0.408 1.006 0.626 1.547 1.153 1.617 0.432
(cm2/cm3)
Specific surface area for fraction 2 < fπ < 50 μm,
LD 0.244 0.260 0.558 0.382 0.913 0.515 0.707 0.275
(cm2/cm3)
Abbreviations: MIP—mercury intrusion porosimetry; DIA—dynamic image analysis; LD—laser
diffraction method.

2.2. Methodology

2.2.1. Experimental Method and the Test Stand

In addition to the tests mentioned in Table 1, mineralogical composition of the soils was
determined by the XRD method using an EMPYREAN X-ray diffractometer from PANalytical.
The degree of pore saturation with water is one of significant factors affecting the soil water
permeability. The elimination of this factor impact is related to performance of tests in apparatus,
which enables carrying out the experiments under total saturation conditions [23]. Because of that,
the permeability coefficient in this study was determined in a triaxial compression chamber, in
accordance with the Head’s methodology (for the first time published in 1982) [24,25] and standards
Water 2019, 11, 2500 4 of 21

found in [26–29]. Triaxial compression apparatus is considered a very precise device, which is
confirmed in the literature, e.g., see [30]. The apparatus consists of three water volume and pressure
controllers, the chamber of triaxial compression apparatus (maximum pressure of 1700 kPa), frame
with load up to 50 kN, an MPX 3000 miniscanner, collecting information from sensors, and a control
computer with specialized software VJ Clisp Studio by the VJ Tech company. The diagram of testing
instruments is presented in Figure 1.

Figure 1. A schematic diagram of the testing apparatus (CP—cell pressure, BP—back pressure, DP—
drain pressure, PWP—pore water pressure, and KCOW—water pressure and volume controller).

2.2.2. Sample Preparation

Samples were formed artificially by compaction in the Proctor apparatus at previously set
moisture content. Then rollers 38 mm in diameter were obtained by means of the Shelby cylinders.
After macroscopic assessment of the core quality, the least disturbed segment was selected and then
a sample of 76 mm in height was cut from it. Samples prepared in this way were placed in a rubber
membrane on the base and were covered from the top with a small dome. A flexible shield covering
the sample was pressed to the base and the dome by four sealing O-rings. Moreover, porous stones
with a permeability coefficient at least 10 times higher than that of the tested sample were placed
between the sample and the aforementioned elements [29]. The chamber was put on the sample
prepared in such a way, which was next filled with deaerated water, that enabled applying isotropic
stresses. The application of various hydraulic pressures to the top and bottom part of the sample
through the dome and base resulted in formation of a hydraulic gradient.

2.2.3. Test Procedure

The applied procedure comprised three stages: saturation, consolidation, and filtration. Stage
one, i.e., saturation, was carried out in two phases:
• phase I—application of a small hydrostatic pressure to the lower base of the sample, so-called
flushing, and
• phase II—pumping deaerated water to the sample via a closed system connected to the sample’s
bottom and top, in a so-called method with the use of two back pressures.
At this stage of testing the pressure in the triaxial chamber and the back pressure were increased
in such a way that the isotropic effective stress in the sample would remain on a constant level during
the entire saturation procedure. An increment of 100 kPa was used, and the amount of this stress was
chosen so as to prevent radial swelling of the soil. Experiments show that, for the studied soils, a
sufficient stress amounted to 10 kPa (i.e., a stress slightly higher than the swelling pressure was
applied). During the saturation, the sample’s height was observed the entire time.
The state of studied soil saturation under conditions of impossible lateral expansion was
estimated based on the value of Skempton parameter B [31], determined from formula [24,27,28]:

Δu
B= , (1)
Δσ
Water 2019, 11, 2500 5 of 21

where: B: Skempton parameter (-); Δu: change of water pressure in pores (kPa), and Δσ: change of
pressure in the chamber (kPa).
Because the parameter B is dependent on soil properties, the saturation process is different in
different soils. In general, the state of full saturation is assumed for the parameter value B = 1.
However, for non-permeable soils (investigated soils), it is justified to assume the state of full
saturation for parameter B ≥ 0.95. The time necessary to obtain such a value for each sample was
approximately 2–3 days.
After the finished stage of saturation, the samples were isotropically consolidated to the value
of effective stresses of approximately 50 kPa. Formulae given by Head [25] were used in calculations:

σ '=σ − ū , (2)

where
σ’: required effective stress (kPa),
σ: isotropic pressure in the chamber (kPa)—in the present study, this is a pressure equal to the last
pressure applied in the saturation phase, i.e., 650 kPa—, and
ū: mean pore pressure calculated based on the formula

2 1
u = × uc + × ub , (3)
3 3
where
ub: pressure at the sample’s top (back pressure) (kPa), and
uc: pressure at the sample’s base (kPa).
At this stage, the excess of water pressure in pores, i.e., the difference between the final constant
pressure of pore water and the back pressure from the last saturation step, was dispersed.
After completed consolidation, the third stage of the study, i.e., filtration, was started. A series
of water-permeability coefficient measurements were performed using two back pressures, at various
values of hydraulic gradient. To this end, pressure differences were used between the top and bottom
base of the sample, ranging from 5 to 45 kPa, which corresponded to hydraulic gradients of 7, 10, 20,
and 30. The values were chosen so as to make the obtained yields reliable. The permeability constant
was determined for the top-down flow. Measurements were carried out at a constant temperature of
22 °C in an air-conditioned room. After the completion of the measurement series, all the results were
exported to the Excel program to perform further calculations.
Knowing the flow, the set gradient, and the sample’s surface area and height, the water-
permeability of soil was calculated based on the formula given below:
𝑄×𝑙
𝑘= (4)
𝐴 × ∆ℎ
where
k—permeability coefficient (m/s),
Q—flow rate (m3/s), l—sample’s height (m),
A—area of sample cross-section (m2), and
Δh—difference of pressures at the sample’s top and bottom (m).

3. Results and Discussion

3.1. Raw Results

The tests of eight soils conducted using the triaxial testing apparatus allowed obtaining the values
of permeability coefficients at four different hydraulic gradient values. The results are shown in Table
3.
Water 2019, 11, 2500 6 of 21

Table 3. Values of flow velocity V and permeability coefficient k obtained for four hydraulic gradients i.

Mean of the
Soil No. i (-) V (m/s) Values k for Individual Tests Mean k (m/s)
Means k (m/s)
6.71 4.65 × 10−9 2.06 × 10−9 2.17 × 10−9 1.92 × 10−9 2.05 × 10−9
Soil no. 1
10.73 8.22 × 10−9 2.32 × 10−9 2.05 × 10−9 2.27 × 10−9 2.21 × 10−9
2.27 × 10−9
20.12 1.69 × 10−8 2.19 × 10−9 2.48 × 10−9 2.43 × 10−9 2.37 × 10−9
30.85 2.70 × 10−8 2.39×10−9 2.29 × 10−9 2.72 × 10−9 2.47 × 10−9
6.71 3.77 × 10−10 6.48 × 10−10 7.40 × 10−10 6.90 × 10−10 6.93 × 10−10
Soil no. 2

10.73 6.59 × 10 −10 7.94 × 10−10 6.98 × 10−10 8.05 × 10−10 7.66 × 10−10
7.93 × 10−10
20.12 1.39 × 10−9 8.09 × 10−10 8.48 × 10−10 8.57 × 10−10 8.38 × 10−10
30.85 2.36 × 10−9 8.19 × 10−10 8.96 × 10−10 9.12 × 10−10 8.76 × 10−10
6.71 5.62 × 10−10 5.69 × 10−11 6.08 × 10−11 5.10 × 10−11 5.62 × 10−11
Soil no. 3

10.73 1.02 × 10−9 6.28 × 10−11 6.53 × 10−11 5.62 × 10−11 6.14 × 10−11
6.58 × 10−11
20.12 2.39 × 10−9 6.21 × 10−11 7.45 × 10−11 7.05×10−11 6.90 × 10−11
30.85 4.41 × 10−9 7.02 × 10−11 8.41×10−11 7.48×10−11 7.64 × 10−11
6.71 1.89 × 10−9 7.88 × 10−11 9.01 × 10−11 8.25 × 10−11 8.38 × 10−11
Soil no. 4

10.73 3.33 × 10−9 8.68 × 10−11 1.063 × 10−10 9.22 × 10−11 9.51 × 10−11
8.94 × 10−11
20.12 6.82 × 10−9 1.28 × 10−10 1.30 × 10−10 9.9 × 10−11 1.19 × 10−10
30.85 1.08 × 10−8 1.35 × 10−10 1.63 × 10−10 1.31×10−10 1.43 × 10−10
6.71 6.84 × 10−9 2.91 × 10−10 2.84 × 10−10 2.72 × 10−10 2.82 × 10−10
Soil no. 5

10.73 1.16 × 10−8 3.10 × 10−10 3.19 × 10−10 3.02 × 10−10 3.10 × 10−10
3.21 × 10−10
20.12 2.33 × 10−8 3.31 × 10−10 3.54 × 10−10 3.32 × 10−10 3.39 × 10−10
30.85 3.67 × 10−8 3.59 × 10−10 3.54 × 10−10 3.40 × 10−10 3.51 × 10−10
6.71 5.23 × 10−10 1.04 × 10−9 1.06 × 10−9 9.6 × 10−10 1.02 × 10−9
Soil no. 6

10.73 9.95 × 10−10 1.06 × 10−9 1.15 × 10−9 1.03 × 10−9 1.08 × 10−9
1.11 × 10−9
20.12 2.01 × 10−9 1.18 × 10−9 1.21 × 10−9 1.09 × 10−9 1.16 × 10−9
30.85 3.79 × 10−9 1.17 × 10−9 1.26 × 10−9 1.14 × 10−9 1.19 × 10−9
Water 2019, 11, 2500 7 of 21

6.71 7.18 × 10−8 7.69 × 10−11 8.18 × 10−11 7.51 × 10−11 7.79 × 10−11

Soil no. 7
10.73 1.15 × 10−7 9.30 × 10−11 9.62 × 10−11 8.89 × 10−11 9.27 × 10−11
9.84 × 10−11
20.12 2.62 × 10−7 1.02 × 10−10 1.06 × 10−10 9.3 × 10−10 1.00 × 10−10
30.85 4.16 × 10−7 1.20 × 10−10 1.31 × 10−10 1.18 × 10−10 1.23 × 10−10
Soil no. 8 6.71 7.18 × 10−8 9.1 × 10−9 1.15 × 10−8 1.06 × 10−8 1.07 × 10−8
10.73 1.15 × 10−7 1.04 × 10−8 1.16 × 10−8 1.01 × 10−8 1.07 × 10−8
1.20 × 10−8
20.12 2.62 × 10−7 1.26 × 10−8 1.24 × 10−8 1.40 × 10−8 1.30 × 10−8
30.85 4.16 × 10−7 1.29 × 10−8 1.44 × 10−8 1.23 × 10−8 1.35 × 10−8
Water 2019, 11, 2500 8 of 21

3.2. Variance Analysis

The variance analysis was carried out using the Statistica 8 software in order to check whether
the results for various soil types and hydraulic gradients i differ from each other in a statistically
significant way. The analysis involved evaluating the independent effect and interactions of the
factors soil and hydraulic gradient on the observed values of permeability coefficients k. The results are
shown in Table 4.
Table 4. Results of the variance analysis.

Degrees Observed
Classifying Predictor of F P Partial η2 Power
Freedom (α = 0.05)
soil 7 1482.217 0.000000 0.993869 1.000000
hydraulic gradient 3 10.241 0.000013 0.324347 0.997706
soil + hydr. gradient 21 59.02 0.000000 0.659452 1.000000

The p-values shown in the Table 4 are the probability that different permeability coefficient k
values (dependent variables) for various groups classified with classifying predictors (independent
variables) have been obtained in a purely random way—that is as a result of difficult to assess
experiment errors. In other words, it is the probability that the so-called null hypothesis is true. The
null hypothesis is the statement that there is no difference among the groups, e.g., different soils have
the same permeability coefficient, or else permeability coefficients obtained for various hydraulic
gradients are equal. The value of 0.05 is usually assumed to be the boundary value of the probability
p.
It can be seen from Table 4 that all p-values are few orders of magnitude smaller than 0.05,
allowing rejection of the null hypothesis. In terms of the current experiments, it can be stated that
both soil type and hydraulic gradient, as well as interaction of these two factors, significantly affect
the obtained values of permeability coefficient k.
Partial η2 (that is the so-called effect size measure, η2 ∈ < 0; 1>) is an indicator determining which
fraction of variability in range of variable A (dependent variable, in our case, k) is explained by
variable B (independent variable, in our case, soil and hydraulic gradient). In other words, partial η2
explains which of the independent variables has greater effect on the results of the dependent
variable. Data in Table 4 show that the type of soil has extremely large impact (partial η2 close to 1).
The effect of hydraulic gradient i is considerably smaller, but it is still statistically significant. It means
that empirical models characterizing the permeability coefficient and taking into account the sole
hydraulic gradient i are reasonable. However, the effect of the gradient in interaction with soil is
bigger than the effect of the sole gradient. This result is in agreement with intuition: The same
gradient in soils of different structures must result in different hydraulic conductivity; in other words,
more permeable soils strengthen the effect of the gradient and vice versa. Summarizing, the measured
values of permeability coefficients depend on the soil type and, to a lesser degree, on the value of
hydraulic gradient. An increasing relationship is observed in the latter case, which can be seen in
Table 4, where mean values for each soil and the hydraulic gradient combination are gathered. The
value of kmean represents “the mean of the means” value, i.e., the values of the permeability coefficient
treated as being independent of the hydraulic gradient.

3.3. Darcianity of the Observed Flows

Data shown in Table 4 and in Figure 2 cannot be treated as settling the issue of Darcianity or
non-Darcianity of the observed flows. Assuming linear relationship between the flow velocity and
the hydraulic gradient as indicative for Darcian flow, we compared two regression models in the
form V = f (i). For the pairs (ij, Vj), linear approximation and non-linear approximation using power,
logarithmic, exponential, and second-order polynomial functions were performed. Among the
nonlinear functions, the best fit was observed for the second degree polynomial (R2 = 1 in all cases).
In Table 5 and in Figures 3 and 4, fitting parameters of linear relationships are shown. These results
Water 2019, 11, 2500 9 of 21

show that the relationship V = f (i) is actually non-linear. It is particularly evident in soils no. 3, 4, and
7. The specificity of just these soils against the others consists in the highest values of the colloidal
activity (1.23, 1.24, and 1.36, respectively). Moreover, soils no. 3 and 7 prove to have highest values
of plasticity index Ip.

2E-08

1E-08

1E-08 Gradient 6.71

Gradient 10.73
1E-08 Gradient 20.12
Gradient 30.85
8E-09
k (m/s)

6E-09

4E-09

2E-09

0E-01

-2E-09
1 2 3 4 5 6 7 8
Soil

Figure 2. The variance analysis results—effect of the interaction soil*gradient on the permeability
coefficient k (vertical bars denote 0.95 confidence interval).
Water 2019, 11, 2500 10 of 21

4.50E-07
Soil 8
y = 1E-08x - 3E-08
R² = 0.9983
4.00E-07

3.50E-07

3.00E-07
Flow velocity (m/s)

2.50E-07

2.00E-07

1.50E-07

1.00E-07 Soil 1
y = 3E-09x - 4E-09
R² = 0.9998

5.00E-08
Soil 6
y = 1E-09x - 2E-09
R² = 0.9999
0.00E+00
0 5 10 15 20 25 30 35
Hydraulic gradient

Figure 3. Fitting of linear function to empirical data V = f (i) for soils nos. 1, 6, and 8.
Water 2019, 11, 2500 11 of 21

3.00E-08

Soil 2
y = 9E-10x - 2E-09
R² = 0.9999

2.50E-08

2.00E-08
Flow velocity (m/s)

1.50E-08

Soil 5
y = 4E-10x - 6E-10
R² = 1
1.00E-08

Soil 4
y = 2E-10x - 6E-10
5.00E-09 Soil 7 R² = 0.9925
y = 1E-10x - 5E-10
R² = 0.9886
Soil 3
y = 8E-11x - 2E-10
R² = 0.9977
0.00E+00
0 5 10 15 20 25 30 35
Hydraulic gradient

Figure 4. Fitting of linear function to empirical data V = f (i) for soils nos. 2–7.

It can be concluded that linear dependence of velocity on hydraulic gradient is an approximation

only, the worse the more cohesive a given soil is. However, as seen in Table 5 and in Figures 3 and 4,
even in the case of the worst fitting (soil no. 7), the linear function can be considered well fitted (R >
0.99427) and highly statistically significant (p < 0.00573). Hence, Darcy’s law is, from an engineering
point of view, a correct approximation of the empirical relationship V = f (i), also in very cohesive
soils.
Water 2019, 11, 2500 12 of 21

Table 5. Fitting parameters of linear relationship between flow velocity and hydraulic gradient.

SS MS SS MS
Sum of Mean Sum of
Soil Mean Squares F Ratio R p Value
Squares Squares Squares
Model Residuals
No. 1 2.32 × 10−15 2.32·× 10−15 4.10·× 10−19 2.05·× 10−19 11327.9 0.99991 0.00009
No. 2 2.98·× 10−16 2.98·× 10−16 3.69·× 10−20 1.84·× 10−20 16197.9 0.99994 0.00006
No. 3 2.34·× 10−18 2.34·× 10−18 5.49·× 10−21 2.74·× 10−21 852.08 0.99883 0.00117
No. 4 8.89·× 10−18 8.89·× 10−18 6.73·× 10−20 3.36·× 10−20 264.35 0.99624 0.00376
No. 5 4.77·× 10−17 4.77·× 10−17 2.02·× 10−21 1.01·× 10−21 47252.6 0.99998 0.00002
No. 6 5.34·× 10−16 5.34·× 10−16 3.15·× 10−20 1.57·× 10−20 33909.4 0.99997 0.00003
No. 7 6.23·× 10−18 6.23·× 10−18 7.20·× 10−20 3.60·× 10−20 172.90 0.99427 0.00573
No. 8 7.32·× 10−14 7.32·× 10−14 1.24·× 10−16 6.18·× 10−17 1185.00 0.99916 0.00084

3.4. Empirical Regression Models

In order to gain a preliminary insight into the data, the Statistica 8 software was used to create
the correlation matrix of averaged permeability coefficient k values with 109 soil parameters,
including: volumetric density of soil; volumetric density of soil skeleton; natural humidity; yield
point (determined using the roll test and cone penetrometer methods); liquid limit (determined using
the Casagrande, Vasiliev, and cone penetrometer methods); plasticity indexes; colloidal activity;
organic matter content; pH value; the proportion of clay, silt, sand, and gravel fractions (measured
using three methods: hydrometer, laser diffraction, and image analysis); reduced fractions calculated
for hydrometer analysis; percentage of pores within ranges: <3 nm, 3–10 nm, >10 nm; total area of
pores; pore size median—measured volumetrically; total mercury intrusion volume; average pore
diameter; volumetric density of pores at the pressure of 3.65 kPa; porosity; void ratio (determined
using the mercury porosimetry method or through calculations); minimum, maximum, and mean
pore area and its medians; minimum, maximum, and mean pore circumference with median (the
NIA Numerical Image Analysis method); shape factors: sphericity, convexity, and shape
proportionality (determined using the image analysis method for silt and sand fraction, and mean
value); total and outside specific surface; approximate montmorillonite content; two sorption
moisture values: w50 and w95 (sorption test method); and specific surface determined relative to the
volume and mass (laser diffraction and image analysis methods for all fractions and mean value).
For the majority of parameters, correlation coefficients (R) are: │R│ < 0.5 (this value indicates poor
correlation). Moderately strong correlations (0.5 < │R│ < 0.7) of permeability coefficients were observed
for the following parameters: liquid limits determined according to Casagrande and cone penetrometer
methods (wLC, wLP), plasticity index (Ip = wLC − wpw), clay and silt fraction (fπ, fi’, fπ’—obtained using the
hydrometer method), pore size median (Mp—the MIP method), minimum pore circumference (Omin—
the NIA method), convexity of particles and particle shape proportionality coefficient for silt fraction
(ψc2–50, ψa2–50—the DIA method), as well as sorption moisture w95, whereas strong correlation (│R│ >
0.7) was observed for these parameters: average pore diameter (Dp—obtained using the MIP method),
and convexity of particles for sand fraction (ψc50–2000—the DIA method).
The complete correlation matrix allowed initial selection of parameters best correlated with
permeability coefficient k (│R│ > 0.5), and those parameters, which were thought to be significant for
filtration phenomenon. Relatively low values of correlation coefficient in the matrix could be
resulting from strongly non-linear dependence for such parameters as the plasticity limit wpw, the
colloidal activity IA, clay fraction content fi obtained using the hydrometer method, porosity and void
ratio obtained using the MIP method (nHg, eHg) or through calculations (nobl, eobl).
The average pore diameter Dp is given by the following equation:

4V
D= , (5)
S
Water 2019, 11, 2500 13 of 21

where
V: pores volume, determined by the mercury intrusion porosimetry (MIP), and
S: pores surface area, determined by the mercury intrusion porosimetry (MIP).
The values of correlation coefficients R for parameters selected in this way are shown in Table 6.
The distinction between “physical” and “structural” parameters here partially is conventional in
character and is partially based on the way in which individual parameters can be obtained. While
the “structural” parameters require more refined techniques, the “physical” ones can be determined
by use of traditional simple methods of soil science. However, the content of clay fraction, for
example, is no less “structural” than pore diameter determined by use of Mercury Intrusion
Porosimetry. On the other hand, models using structural parameters as difficult to obtain as the
permeability coefficient itself seem less practical, though they could have theoretical significance in
understanding the nature of the transport processes in porous media.

Table 6. Values of correlation coefficient R with permeability coefficient k for the best correlated
parameters.

Parameter Correlation Coefficient

Parameter
Type with k
physical plastic limit wP −0.146703
physical liquid limit by use of Casagrande’s method wLC −0.504481
physical liquid limit by use of cone penetrometer method wLp −0.501565
physical plasticity index Ip = wLC − wp −0.535338
physical colloidal activity IA −0.461156
physical clay fraction by use of hydrometer method CF’ −0.499554
physical silt fraction by use of hydrometer method SF’ 0.568840
physical reduced clay fraction by use of hydrometer method CF’ −0.500901
physical reduced silt fraction by use of hydrometer method SF’ 0.579682
physical calculated porosity ncalc 0.160608
physical calculated void ratio ecalc 0.140694
physical sorption moisture at p/p0 = 0.95 w95 −0.514057
structural pore size median by MIP Mp 0.616287
structural average pore diameter Dp 0.941742
structural porosity by use of MIP nHg 0.456891
structural void ratio by use of MIP eHg 0.430623
structural minimum pore circumference by use of NIA Omin 0.604273
particle shape proportionality coefficient for silt fraction
structural −0.597394
ψa2-50
structural convexity particles for silt fraction ψc2-50 0.630566
structural convexity of particles for sand fraction ψc50-2000 −0.735984

Then, the selected parameters were used to create empirical models characterizing permeability
coefficient k. The Levenberg–Marquardt non-linear estimation method was applied for that purpose.
The empirical models were determined using the following functions:
• power:

k = a1 × x a2 , (6)

• logarithmic:

k = a1 ln( x) + a2 , (7)

• exponential:
Water 2019, 11, 2500 14 of 21

k = a1 exp(a2 × x) , (8)

where

x: analyzed soil parameter, and

a1, a2: estimators of model parameters.
The values of correlation coefficients R for the models are shown separately for physical and
structural characteristics in Tables 7 and 8. The highest values are printed in bold and red.

Table 7. The values of correlation coefficient R for one-parameter models with one physical
parameter.

Function Correlation Coefficient with Parameter

Type wp wLC Ip A CF’ SF’ ncalc ecalc w95
power 0.081 0.899 0.995 0.315 0.992 0.459 0.000 0.133 0.396
logarithmic 0.105 0.580 0.763 0.416 0.648 0.449 0.179 0.171 0.638
exponential 0.125 0.987 0.992 0.381 0.992 0.974 0.124 0.107 0.989

The correlation coefficient values allowed finding the best fitted models with one parameter for
both of the above-mentioned groups of physical and structural parameters. According to Table 7, the
highest values of the coefficient R are observed for the following parameters: Ip (R = 0.99499, power
function), CF’ (R = 0.99238, power function), w95 (R = 0.98919, exponential function), wLC (R = 0.98679,
exponential function), and SF’ (R = 0.97368, exponential function), whereas, according to Table 8—
for Dp (R = 0.98752, power function)—, ψc2–50 (R = 0.98591, power function). Table 9 presents specified
estimators of parameters a1, a2 for the best-fitted models with the corresponding statistical
significance values and confidence intervals.

Table 8. The values of correlation coefficient R for one-parameter models with one structural
parameter.

Correlation Coefficient with Parameter

Function Type
Mp Dp nHg eHg Omin ψc2–50 ψc50–2000
power 0.642 0.988 0.437 0.418 0.599 0.986 0.211
logarithmic 0.475 0.659 0.451 0.452 0.599 0.621 0.739
exponential 0.475 0.475 0.394 0.345 0.599 0.364 0.130

Table 9. The values of estimators of model parameters with the corresponding statistical significance
values and confidence intervals for physical and structural parameters (the symbol in column
“Function Type” identifies the functions: P—power; E—exponential).

Parameter Function Statistical Lower Limit of Upper Limit of

Estimator
Type Type Significance p Confidence Interval Confidence Interval
a1 1.48·× 10−6 0.00000 1.48·× 10−6 1.48·× 10−6
Ip P
a2 −2.93561 0.00000 −3.63508 −2.23613
a1 0.00217 0.57022 −0.00668 0.01103
CF’ P
a2 −6.19169 0.00033 −8.26441 −4.11896
physical

a1 0.00002 0.41886 −0.00003 0.00006

w95 E
a2 −3.83447 0.00078 −5.33666 −2.33229
a1 0.07439 0.69346 −0.36561 0.51439
wLC E
a2 −0.77539 0.00143 −1.11689 −0.43389
a1 3.69·× 10−14 0.00000 3.69·× 10−14 3.69·× 10−14
SF’ E
a2 0.19324 0.00000 4.71·× 10−2 0.33935
a1 2.09·× 10−9 0.00000 2.09·× 10−13 2.09·× 10−13
structural

Dp P
a2 1.85356 0.00000 1.28509 2.42203
a1 4.88·× 10−19 0.00000 4.88·× 10−19 4.88·× 10−19
ψc2−50 P
a2 −2.04·× 10−2 0.00000 −2.04·× 10−2 −2.04·× 10−2
Water 2019, 11, 2500 15 of 21

The models with structural parameters do not prove to be better fitted than the models with
physical parameters. Presumably, this is the result of the effect of the “non-structural” factors, in
particular capillarity and the bound water properties. They are strongly related to such physical
parameters as the plasticity index, the clay fraction content, sorption moisture w95, and the colloidal
activity. These facts allow an important general conclusion: it is not possible to effectively model the
water flow in poorly permeable soils using structural data only, related with the volume, size, and
shape of pores or particles.
The values of estimators statistically significant at p < 0.05 are printed in bold and red. Parameter
estimators of the models with CF’, w95, wLC appear statistically insignificant at the 0.05 level. In turn,
the model with silt fraction SF’ is characterized by the least correlation coefficient of all the models in
Table 9. Taking into account the above, the following empirical model with one physical parameter
is proposed:

k = a1 × I p a2 →R = 0.99499, (9)

where

Ip: plasticity index calculated from Ip = wLC − wpw (%), and

a1 = 1.48·× 10−6, a2 = −2.93561.
The following empirical models with one structural parameter are proposed:

k = a1 × D p a2 → R = 0.98752, (10)

where

Dp: average pore diameter obtained using the MIP method (nm),
a1 = 2.09·× 10−14, a2 = 1.85356,
or

k = a1 ×ψ c 2−50 a2 →R = 0.98591, (11)

where:

ψc2–50: convexity of particles for silt fraction obtained using the DIA method (-), and
a1 = 4.88·× 10−19, a2 = −2.04·× 10−2.

3.5. Models Validation

Four common metrics were used in the validation process for measuring the differences between
permeability coefficient values predicted by the proposed models and the values observed: Mean
Absolute Error (MAE), Mean Bias Error (MBE), Mean Absolute Percentage Error (MAPE), and Root-
Mean-Square Error (RMSE). The results are compared with results obtained by use of two frequently
used models from references, among others, such as equation based on the void ratio e, plasticity
limit wp, plasticity index Ip [17].
Water 2019, 11, 2500 16 of 21

.
𝑒 − 0.027 × (𝑤 − 0.242 × 𝐼 )
0.074 ×
𝐼 (12)
𝑘=
1+𝑒
and, on the void ratio, the percentage of clay fraction fi, and the colloidal activity IA [18]:

𝑒 1
× (13)
𝑓𝑐 𝐼𝐴 + 1

The calculations using Equations (12) and (13) were done for three sets values of the void ratio,
i.e., obtained by use of MIP (eHg) calculated from the dry density and the specific gravity (ecalc) and the
void ratio in the saturated state (ecalc). In the cases of both equations, ecalc yielded the best fitting to
experimental data, and these results are presented further by default.
In Table 10, values of the above listed metrics are presented for Equations (9)–(13).

Table 10. Measures of fitting models given by Equations (9)–(13).

Model MAE (m/s) RMSE (m/s) MAPE (%)

Equation (9) 3.17 × 10−10 4.35 × 10−10 68.56
Equation (10) 5.66 × 10−10 7.03 × 10−10 150.41
Equation (11) 7.64 × 10−10 9.77 × 10−10 338.32
Equation (12) 1.64 × 10−9 3.59 × 10−9 51.68
Equation (13) 4.27 × 10−9 4.88 × 10−9 59.35

Figure 5 represents scatter plot for values observed and calculated using the five analyzed
models. Data scattering for the three most impermeable soils with k < 1 × 10−9 m/s (nos. 2–5) is more
conveniently presented in the inlay.
Water 2019, 11, 2500 17 of 21

Eq. (9) Eq. (10) Eq. (11) Eq. (12) Eq. (13)
1.E-08

1.E-08
Calculated permeability coeffcient (m/s)

1.E-08

8.E-09

6.E-09

4.E-09

2.E-09

0.E+00
0.00E+00 2.00E-09 4.00E-09 6.00E-09 8.00E-09 1.00E-08 1.20E-08 1.40E-08
Observed permaebility coefficient (m/s)

Figure 5. Scatter plot for the values observed and calculated using the five analyzed models.

It is apparent from data shown in Table 10 and in Figure 5 that the observed values are estimated
by the multivariable models given by Carrier and Beckman [17] and Mesri et al. [18] with sufficient
accuracy, though they turned out worse than expected in terms of MAE and RMSE. Both models
yielded similar values of MAPE (52% and 59%, respectively). However, the precision of one of the
proposed single-variable models (Equation (9) basing on the plasticity index Ip) is quite comparable.
Moreover, the single-variable model turns out to be better in terms of two metrics, i.e., MAE and
RMSE, showing slightly less fitting with regard to MAPE. Both MAE and RMSE express average
fitting error of model in units of the variable of interest, here in (m·s−1). Because permeability
coefficient values of most cohesive soils are not less than several 10−10 m·s−1, the average fitting error
on the level of 3 × 10−10 to 4 × 10−10 m·s−1 certainly is acceptable, as not changing the order of magnitude
of the estimate. In contrast, the values of MAE and RMSE obtained for the reference models suggest
a possibility of error bigger than the order of magnitude of the observed value. Similarly, the model
by Carrier and Beckman yielded two orders of magnitude underestimated result for soil no. 5. Being
almost pure kaolinite, this soil is characterized by an “untypical” set of properties (e.g., for such a
high values of the plastic limit and the content of clay fraction, the void ratio is expected to be higher
than the one observed).
With regard to individual soils, the model with Ip is best fitted for soils no. 1 and no. 8 (i.e., the
minimum absolute value of the difference between the observed and the estimated values for this
soils was obtained by use of just this model), the model with D is best fitted for soil no. 5, the model
with convexity for soil no. 6, the model of Carrier and Beckman for soils nos. 3, 4, and 7, and the
Water 2019, 11, 2500 18 of 21

model of Mesri et al. for soil no. 2. Interestingly, it is possible to indicate characteristic features for
most of soil subgroups separated in this way. Soils no. 1 and no. 8 are characterized by minimum
values of both the liquid limit wL and the clay fraction content fc, minimum specific surface area of
particles between 2 and 50 μm and maximum value of the average pore diameter Dp. Soil no. 5
possesses minimum value of colloidal activity IA, which results from its mineralogical composition
(kaolinite). Structurally, this soil is characterized by maximum void ratio ecalc and porosity ncalc and
minimum values of such particle characteristic as sphericity, aspect ratio, and convexity. Soils no. 3
and no. 7 have maximum values of the liquid limit wL and the colloidal activity IA, minimum values
of the void ratio ecalc, and low value of the average pore diameter Dp. Soil no. 4 is characterized by
minimum value of the plastic limit wP and big value of the colloidal activity.
Soil no. 6, for which the model with convexity shows the best fitting, does not show any special
features in terms of the measured physical and structural parameters. Apparently, convexity of the
silt fraction of particles is a very important structural parameters, negatively related to the
permeability coefficient. Convexity, being the ratio of the perimeter of an object’s convex hull to the
perimeter of the object itself [32], corresponds to a “smoothness” of the silt particles. A small value of
convexity implies a more intensive jamming of particles, which results in reducing the area allowing
water flow. Such a phenomenon, however, concerns only the permeability coefficient, and is not in a
significant relation to other physical or structural parameters of soil (negative correlations observed
with the compact density and the so-called effective density determined by use of mercury
porosimetry speak in favor of such a thesis).
In turn, the worst-fitting models compared to others for a given soil are as follows: for soils nos.
3, 4, and 7—the model with convexity; for soils nos. 2 and 6—the model with the average pore
diameter; for soil no. 8—the model of Mesri et al.; and for soils nos. 1 and 5—the model of Carrier
and Beckman. Summarizing, the models with single structural parameter turn out the worst for 5
soils out of 8. This fact suggests low usability of such models; it is not probably possible to predict
the permeability coefficient basing on structural parameters only. Structural parameters describe the
pore space and as such are evidently important at modeling the flow phenomena in porous media.
However, the real flow strongly depends also on properties related to water and its interaction with
mineral and organic particles, i.e., the degree to which water is “bound” in the system (including the
water adsorbed on mineral surface and the water confined in pores), the average thickness of
conventional layers of the adsorbed water, the amount of amorphous colloidal silica gel, the extent
of capillary condensation, and many others. As rightly stated in [33], “modeling the transport of
fluids in charged multiscale materials, such as clay, is a challenge because it is limited by the smallest
pores, with sizes in the 1–100 nm range, where interfacial effects, such as wetting or electrokinetic
couplings, play a dominant role. Under confinement down to the nanometer scale, one should also
expect the departure from continuous hydrodynamics”. Moreover, in [16], a thesis is presented that
IP “may represent to some extent the shape of the pores and the fabric of the soil”. It seems information
on most of these factors is contained in the plasticity index, a value being the difference between the
liquid and plastic limits and, as such, determining the size of the range of water contents where the
soil exhibits plastic properties. The connection of this parameter to the permeability coefficient is
widely known, yet the fitting quality of the presented single parameter model is in some way
surprising. However, it must be stressed that validity of Equation (9) is limited to the range of the
plasticity index of the tested soils, i.e., between 5 and 55%. A possibility of extrapolation is highly
doubtful.
Going back to the multi variable reference models, it must be stressed that all of them, together
with many models not discussed here [19,20], use porosity as one of the main parameters. The
importance of this soil property seems intuitively obvious, however, the matter is not so simple. As
shown results presented in this study, the average pore diameter, rather than overall amount of pores,
governs the water flow in a porous medium. This statement appears particularly significant in
cohesive soils, for which the porosity and the void ratio strongly depend on the water content. It is
not clear what values of the void ratio the authors of these models have in mind. For example, the
model of Carrier and Beckman [17] is very sensitive to small changes in the void ratio value.
Water 2019, 11, 2500 19 of 21

Meanwhile, this parameter often is biased and, what is worse, depends heavily on the water content.
The conditions in which the seepage will occur are hard to predict in advance, therefore, it is
impossible to know the proper value of the void ratio. Similarly, authors of the model presented in
[19] stated that their model allowed them “to predict the hydraulic conductivity k (m/s) of non-
swelling or limited-swelling clays”. However, the authors give results for two soils at various void
ratio values, the latter resulting most likely from swelling. In the present study, this model shows
acceptable fitting for the void ratio values in saturated state, determined prior to experiment, yet the
results were overestimated. Probably there are “the best” void ratio values enabling one to obtain
best fitting, but such a procedure makes no sense. The same applies to other models using porosity
as the main parameter. Paradoxically, what we predict and what is the permeability coefficient
specific for a given soil is not sufficiently defined. The parameter in question is very sensitive to the
transitory state of soil on one hand and to experimental conditions on the other.
Independently of possible practical usefulness of the model given by Equation (9), allowing to
quickly estimate the permeability coefficient of saturated fine grained soils, the relation is of
theoretical importance, quantitatively showing the strong dependence of the permeability coefficient
on soil plasticity. Similarly, good fitting of the model given by Equation (10) indicates the crucial
significance of the mean pore size in contrast to frequently used parameters describing relative
amount of pores, i.e., the porosity and the void ratio. In our opinion, this fact should be taken into
account during further workings on soil permeability models. Finally, the surprising quality of the
model with convexity Equation (11) may be an important clue for soil researchers using modern
techniques allowing one to identify shape characteristics of pores and particles. It is hard to identify
the most significant characteristics “in advance” using a purely conceptual approach. However,
despite the issues generated by reference models for some tested soils, there is no doubt that only the
description of filtration by two- or multi-parameter models are able to be used as fail-safe predictive
tools.

4. Conclusions
• It has been confirmed that Darcy’s law is not a fully precise description of the flow in poorly
permeable soils, yet the linear dependence between flow velocity and hydraulic gradient is a
good approximation of actual phenomena (R ≥ 0.99427). Statistical relationships have been found
between physical and microstructural parameters and the permeability coefficient of poorly
permeable soils.
• No significant correlations of the permeability coefficient with frequently used soil parameters
describing relative amount of pores were found.
• The model with plasticity index IP turned out to be best fitted to experimental data.
• The structural parameters most correlated with the permeability coefficient are the average
pores diameter DP (determined by the use of mercury intrusion porosimetry MIP) and convexity
of silt particles Ψ2-50 (between 2 and 50 μm, determined by the use of dynamic image analysis
DIA).
Author Contributions: conceptualization, T.K.; methodology, A.L.; validation, T.K. and A.L.; formal analysis,
T.K.; investigation, A.L.; resources, A.L.; data curation, A.L.; writing—original draft preparation, T.K and A.L.;
writing—review and editing, T.K.; visualization, T.K. and A.L.; supervision, T.K.

Funding: The project is supported by the program of the Minister of Science and Higher Education under the
name: “Regional Initiative of Excellence” in 2019–2022 project number 025/RID/2018/19.

Conflicts of Interest: The authors declare no conflict of interest.

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