A LABORATORY CHARACTERIZATION OF SOILS

AND CLAY-BEARING ROCKS USING THE ENSLIN-

NEFF WATER-ADSORPTION TEST
ANA PETKOVS̆EK, MATEJ MAC̆EK and BOJAN MAJES

About the authors 1 INTRODUCTION

Ana Petkovšek
University of Ljubljana, A test method for determining the water-adsorption
Faculty of Civil and Geodetic Engineering capacity of powders was proposed by Enslin in 1933.
Jamova 2, 1000 Ljubljana, Slovenia It was found to be applicable to viscous silk, cellulose,
E-mail: [email protected] paint, glue, gelatine, adhesives based on starch, soils
and some other substances. The method has, however,
Matej Maček been improved several times since then [1]. Today,
University of Ljubljana, the method is included in the German industrial
Faculty of Civil and Geodetic Engineering norm DIN 18 132 [2], and is known as the Enslin-Neff
Jamova 2, 1000 Ljubljana, Slovenia
water-adsorption test (wA). The test is widely used in
E-mail: [email protected]
clay mineralogy and in the production of bentonite for
quality control [3]. Although the Enslin-Neff method
Bojan Majes
University of Ljubljana, is simple, quick to perform, inexpensive and can give
Faculty of Civil and Geodetic Engineering important information about the nature and the behav-
Jamova 2, 1000 Ljubljana, Slovenia iour of geological materials, practically no results have
E-mail: [email protected] been published about the physical meaning of Enslin-
Neff water-adsorption values for real soils and clay-
bearing rocks. Available publications, mostly published
Abstract by German researchers, deal with improvements to the
method [4], [5], the reproducibility of the results [1],
The application of the Enslin-Neff water-adsorption test
and the comparability of the results with the Atterberg-
for the determination of soil-index properties has been
limits values [6]. Dieng [6] investigated natural soils,
investigated on commercially available reference minerals
bentonites and kaolinitic clays, and laboratory-prepared
and on real soils. The Enslin-Neff test is a simple and
mixtures of kaolin and bentonite with limestone, as well
reliable laboratory method, which can provide important
as laboratory-prepared mixtures with lime and organic
information about the behavior of soils, clay-bearing
material in order to define the relationship between the
rocks and aggregate fines that are in contact with water.
water-adsorption value and the Atterberg-limits values
Although the test has been frequently used for bentonite
(wL and IP). Based on the results of his experiments, he
testing, practically no results have been published about
defined the relationships between the wA and wL and IP
the physical meaning of the Enslin-Neff water-adsorption
values as follows:
values for real soils. The results of this study indicate
that the Enslin-Neff water-adsorption test can be used to For soils with:
obtain accurate values of some soil-index properties, such
as the liquid limit, the plasticity index, the methylene-blue w A + 0.3 w Ai ≤ 210% (1)
value, and the soil-water characteristic curve.
w L = 0.61(w A + 0.3 w Ai ) (2)

when: wA > 40%

Keywords
water adsorption, methylene blue value, soil water I P = 0.28(w A + 0.3 w Ai ) − 5 kaolin (3)
characteristic curve, soil suction
I P = 0.51(w A + 0.3 w Ai ) −13 other soils (4)

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A. PETKOVS̆EK ET AL.: A LABORATORY CHARACTERIZATION OF SOILS AND CLAY-BEARING ROCKS USING THE ENSLIN-NEFF WATER-ADSORPTION TEST

For soils with: For the purpose of this study, the readings after 24 hours
were used as a reference for all three bentonites.
w A + 0.3 w Ai > 210% (5)

w L = 1.13(w A + 0.3w Ai ) −126 (6)

I P = 1.1(w A + 0.3 w Ai ) −140 (7)

Dieng [6] defined the value of wAi as a function of water

adsorption after 100 minutes (wA100) and water adsorp-
tion after 5 minutes (wA5):
Figure 1. The Enslin-Neff device used in the experiment.
w Ai = w A100 − w A5 (8)
The Atterberg-limits test was determined according to
Compared with the Atterberg-limit values for soil clas- the standard SIST TS CEN ISO/TS 17892-12:2004 [8].
sification, the advantage of the Enslin-Neff method is that For the determination of the liquid limit a 60g/60° cone
only a very small sample, about 3 grams, is needed for was used. The reference samples were used in the natural
the test. This means that the test could be used to identify state, without sieving, whereas in the case of the real
the nature of soils, rocks and aggregate fines even in cases soil and clay-bearing rocks, only fines passing through a
when other test methods cannot be used due to the lack 0.063-mm sieve were used.
of samples of an adequate size, for instance when study-
ing fine-layered or fractured expansive clay-bearing rocks The methylene-blue value, expressed as MBf , was deter-
and the slip surfaces of rocks, when testing the nature of mined using the standard method defined in SIST EN
fines in the aggregate production industry, for forensic 933-9:1999 [9]. The qualitative mineralogical composi-
and other purposes. tion was determined by X-ray diffraction analysis using
a Phillips device with Cu Kα radiation.
This paper presents the results of a study in which the
results obtained for the Enslin-Neff water adsorption The soil suction at low suction rates was determined by
(wA) were compared with those obtained by a test of the the axial-translation technique, using a soil-moisture
Atterberg limits (wL, IP), the methylene-blue test (MBf), pressure-plate device. Saturated samples that had been
and the soil-suction measurements for determining the prepared at a water content equivalent to the liquid
soil-water characteristic curve (SWCC) [7]. limit or slightly higher were placed on a porous plate
with a high air-entry value, and then maintained at the
chosen cell air pressure of 10 kPa, 33 kPa and 100 kPa.
2 METHODS At suction rates higher than 100 kPa, a Decagon chilled-
mirror dew-point potentiometer was used for the tests.
Water-adsorption values were determined according to
the German norm DIN 18 132 [2] using a conventional
Enslin–Neff device (Figure 1). Oven-dried samples with 3 MATERIALS
weights of 0.3 grams, in the case of bentonites, and 1 gram
in the case of other powders, were placed on the frit using For the purpose of this study, 134 samples were prepared
the recommended funnel method. For each material in and tested. The five reference samples consisted of
the experiment, three parallel tests were performed in commercially available materials: non-active limestone
order to check the reproducibility. The readings of the flour, brick clay and Na+ and Ca2+ bentonites. All the
burette were recorded continuously, with the first read- other samples were taken from typical Slovenian soils
ing after 15 seconds, and then following the power law. and clay-bearing rocks, and consisted of mixtures over
The final reading was taken after 24 hours. The effect of a wide spectrum of different minerals: Eocene flysch
evaporation from the burette was determined prior to the marl and claystone, Oligocene highly overconsolidated
experiment. With the increasing duration of the test the grey marine clay and marl, Miocene marl, Pliocene
effect of evaporation on the readings increases. For most overconsolidated clays from the Sub Pannonian basin,
of the soil samples in the experiment, the water uptake in and Pliocene karstic clays (terra rosa). Quaternary allu-
the sample was finished after 15 minutes. For the reference vial and delluvial soils, taken from weathered zones in
bentonites the readings lasted for more than 24 hours, so alluvial gravels, carbonatic, ultramafic and metamorphic
that the error due to evaporation could be relatively large. phyllonites were also included in the test program.

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 A. PETKOVS̆EK ET AL.: A LABORATORY CHARACTERIZATION OF SOILS AND CLAY-BEARING ROCKS USING THE ENSLIN-NEFF WATER-ADSORPTION TEST

Table 1. Characteristics of the soils used in the research.

Sample wL IP wA MBf ws1500kPa Dominant mineral*

% % % g/kg %
Bentonite Wyoming 535 490 778 336 MNa
Bentonite Macedonia 207 172 297 176 46 MCa
Bentonite Slovenia 83 56 113 172 MCa
Brick clay Slovenia 53 36 73 57 14 I/C
Stone flour Slovenia 23 - 32 2 1 Ca, CaCO3: 99 %
Oligocene marine clay 41-48 26-29 62-70 48-25 11-12 MM:I/K/Ca/Q/
Eocene flysch 42-50 25-32 56-64 56-60 11–13 MM: I/K/Calc/Q/
Miocene marl 39-53 15-34 56-74 20-31 7-11 MM: I/K/M/Calc/Q/
Pliocene clay 52-85 25-57 67-88 61-62 11-23 MM: I/K/M/Q/mica
Pliocene karstic clay 63-122 41-89 83-121 8-13 20-35 L/Mn/Ca/Q
Alluvial clay 67-68 49-51 78-82 38-40 14-15 MM: I/K/M/Q
W – gravel river alluvium 37-42 8-16 47-55 3-12 3–7 MM
W - dolomite 21-38 6-20 29- 51 2–34 2-11 MM: D/I/C
W – phyllonite 27-40 8-19 41-57 7-11 3-9 MM:Sc/C/B/Q
W – serp. harzburgite 40-78 19-42 68-116 28 13-16 S/C/L/O
* MNa – Na montmorillonite > 70 %; MCa – Ca montmorillonite > 70 %, I- illite/muscovite, B – biotite, C – chlorite, Ca – calcite, D – dolomite, L – limonite,
MM – wide mineral mixture, Mn – manganese oxide, O – olivine, Q – quartz, S – serpentinite, Sc – sericite, W – weathered products inside the bedrock

The liquid limits and the plasticity indexes of the tested

4 RESULTS AND DISCUSSION soils are presented for all the samples in Figures 2 and 3.
The reference samples (commercially available materi-
The results for the Atterberg-limit values, the Enslin-Neff
als) are indicated in the key in each diagram. The refer-
water absorption, the methylene blue, the water content
ence clayey samples were found to be located close to
at a soil suction equal to 1500 kPa and the prevailing
the same straight line, which corresponds to the U-line
mineral composition are given in the ranges for the repre-
in the AC diagram, whereas most of the tested real soils
sentative samples of the typical groups of soils (Table 1).

Figure 2. Position of the tested soils in the AC diagram, limited scale (left) and complete scale (right).

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A. PETKOVS̆EK ET AL.: A LABORATORY CHARACTERIZATION OF SOILS AND CLAY-BEARING ROCKS USING THE ENSLIN-NEFF WATER-ADSORPTION TEST

lie above the A-line (Figure 2). The U- and A-line are For the real soils, the values of the coefficient in equation
defined as in the ASTM standard D 2487-00 [10], where (10) can vary between 1.13 and 1.77. The experimentally
the U-line is defined as the empirically determined defined relationship is close to that proposed by Dieng
approximate “upper limit” for the natural soil and the [6], but it is expressed in a much simpler form.
A-line as the border line between silts and clays.
For the real soils the scattering of the results seems to
increase with the increasing liquid limit (Figure 3).
4.1 RELATIONSHIP BETWEEN THE Therefore, the coefficient wA/wL was calculated for all the
ENSLIN-NEFF WATER-ADSORPTION samples and the standard deviation was determined to be
TEST AND THE ATTERBERG-LIMITS 0.2. Figure 4 presents the distribution of the coefficient
TEST wA/wL and the normal distribution for the determined
standard deviation and coefficient wA/wL. The liquid limit,
The Atterberg-limits test is one of the most widely wL, could be calculated with a 10% accuracy from the real
used tests in soil mechanics for classification purposes, measurement by using equation (10) for more than 50% of
although it is partially subjective and requires experi- the samples (for example, wL=40% in the range 36–44%).
enced laboratory staff. At least 200 g of soil is needed for
the test, which is quite inconvenient, especially when
thin layers of highly expansive clay are encountered
inside the bedrock mass or when coarse material with a
low fines content has to be tested. However, the Enslin-
Neff test is a promising test that could overcome the
shortcomings of Atterberg’s soil-classification test.

The experimentally determined relationship between

the Atterberg liquid-limit test and the Enslin-Neff water-
adsorption test is given in Figure 3.

For the reference materials an excellent correlation was

found between wA and wL and the corresponding simple
equations can be written as:

w L = 0.69 w A (9)

w A =1.45 w L (10) Figure 4. Grouping of the soils following the position in the
AC diagram.

Figure 3. Enslin-Neff water adsorption as a function of the liquid limit, limited scale (left) and complete scale (right).

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 A. PETKOVS̆EK ET AL.: A LABORATORY CHARACTERIZATION OF SOILS AND CLAY-BEARING ROCKS USING THE ENSLIN-NEFF WATER-ADSORPTION TEST

Figure 5. Grouping of soils following the position in the AC diagram (left) and the relationship wL–wA (right).

To explain the influence of the different types of soils The results of the experiments show that both values,
on the ratio wA/wL, the samples were divided into four i.e., wA and wL, have similar physical meanings when
groups: lean clays and silts represent a special group with describing the clean mono-mineral soils as well as
a liquid limit wL < 30%, whereas the groups R1, R2 and the real heterogeneous soils. In the case of both tests,
R3 were defined according to the soil position in the AC the measured water content belongs to the water
classification diagram (Figure 5). adsorbed to the external and internal surfaces of the
grains. However, the water content at the liquid limit
From Figure 5 it can be concluded that the type of soil does
corresponds to an undrained shear strength of cu = 1.6
not influence the relationship wA/wL and that equation (10)
kPa [11], but does not correspond to the maximum void
is valid for all types of soils. However, for the relationship
ratio (emax). The sample on the frit in the Enslin-Neff
between wA and IP (Figure 6) these findings are not valid.
device is in the loosest state, and is completely saturated
when the test is finished. The water content obtained
from the Enslin-Neff test is therefore higher than the
water content at the liquid limit for the specific soil.

The results of the experiments also confirmed that the

Enslin-Neff method could replace or provide an excel-
lent complement to the liquid-limit test, especially in
cases when limited quantities of samples are available for
the test, or when it is difficult to perform the liquid-limit
test, as in the case of Na+ bentonites or low plastic soils
and micas.

4.2 RELATIONSHIP BETWEEN THE

ENSLIN-NEFF WATER-ADSORPTION
TEST AND THE METHYLENE-BLUE
VALUE
It is well known that the specific surface area (SSA) and
the cation-exchange capacity (CEC) influence the behav-
iour of clay in contact with water and water solutions.
Figure 6. The index of plasticity as a function of water adsorp- For more than 40 years the methylene-blue (MB) test has
tion and soil group. been recognized as a rapid and easily applicable test for

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A. PETKOVS̆EK ET AL.: A LABORATORY CHARACTERIZATION OF SOILS AND CLAY-BEARING ROCKS USING THE ENSLIN-NEFF WATER-ADSORPTION TEST

SSA and CEC determination [12], [13], [14], [15], and function with a correlation coefficient of R2 = 0.54. The
different classification charts for predicting the swelling correlation coefficient was only calculated for the real
potential of soils are based on MB values [13], [15], [16]. soils. The reference bentonites were not included, since
In its aqueous state methylene blue is a cationic dye, the small number of these samples with positions far
C16H18N3S+, which can adsorb onto negatively charged away from the centre of the group would have drastically
surfaces. The MB molecule has a rectangular shape with improved the correlation coefficient R2.
the dimensions 17 Å*7.6 Å*3.25 Å, and it is assumed
that the MB molecule lies on its largest surface [15]. No However, in the literature it has been reported that the
special equipment is needed for the test. The MB value is MB shows a high dependency of the adsorption on the
determined by measuring the quantity of methylene-blue type of cations in/on the clay. Researchers have reported
dye necessary to cover the total (external and internal) that the adsorption of the MB dye is only complete when
surface area of the particles contained in the soil. the sample is in the lithium and sodium exchanged form
[15]. From this point of view it is too early to recognize
From this point of understanding, the Enslin-Neff and the Enslin-Neff test as a method that could successfully
the MB tests exploit similar phenomena – the adsorption replace the MB test, but it can certainly complement it.
of water molecules or positively charged dye cations onto The results of the research are promising and show that
negatively charged external and internal particle surfaces. It these investigations should be continued, taking into
can therefore be assumed that the correlation between the account the influence of the specific cation-exchange
MB and Enslin-Neff must exist in soils that contain nega- capacity and the specific surface area of the tested soils
tively charged surfaces, and where the amount of adsorbing on both of the measured parameters.
water prevails over the amount of capillary water.

The experimentally determined relationship between the 4.3 ENSLIN-NEFF WATER ADSORPTION
MBf and wA values is given in Figure 7. It can be seen that – SWCC
there is no unique and linear relationship between the
two measured parameters, which is probably due to the The soil-water characteristic curve (SWCC) is a continu-
influence of the capillary water and of the different sizes ous sigmoidal function, represe nting the relationship
of the adsorbing molecules. The concentration of the between the water content (gravimetric or volumetric)
results at lower values of MBf (MBf < 15g/kg) belongs to or the saturation degree and the stress state of the pore
the silty soils (group R1), where most of the water in the water. Many soil properties can be related to SWCC,
soil belongs to the capillary water and the particles can be such as the volume change, the hydraulic conductivity
estimated as inert. At values of MBf > 15g/kg the correla- and the shear strength. The SWCC has three stages that
tion between MBf and wA can be expressed as a potential describe the process of desaturation of a soil: the capil-

Figure 7. The MBf – wA relationship, limited scale (left), complete scale (right).

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 A. PETKOVS̆EK ET AL.: A LABORATORY CHARACTERIZATION OF SOILS AND CLAY-BEARING ROCKS USING THE ENSLIN-NEFF WATER-ADSORPTION TEST

lary saturation zone, where the pore water is in tension similarity with the saturated soil oedometric compres-
but the soil remains saturated due to capillary forces; the sion curve, the “virgin” SWCC.
desaturation zone, where the water is displaced by air
within the pores; and the residual saturation zone, where The laboratory tests for SWCC determination at low
the water is tightly adsorbed onto the soil particles and suction usually start on samples that have been prepared
flow only occurs in the form of vapour [7]. at the liquid limit, which means that the soil is no longer
in the loosest state. Following the description of Dieng
The capillary saturation zone ends at the air-entry value, [6], the Enslin-Neff water adsorption can correspond
where the applied suction overcomes the capillary water to the first point on the “virgin” SWCC at which the
forces in the soil and air enters the pores. The amount of soil pores and the diffusive double layers are filled with
water in the soil or the water content at a certain suction water. A relationship between the water content at zero
stress depends on the soil’s density and the soil’s stress suction and the water content at the residual water
history. However, each type of soil has a characteristic content must therefore be expected.
maximum void ratio in its loosest state (emax), at which
it can hold the highest amount of water in the saturated Figure 8 shows the SWCC curves of four representative
state (at zero suction). This point corresponds to the first soils used in the investigation. For each soil sample the
point on the SWCC, which can be called, following the experimentally determined soil suctions are given for

Figure 8. SWCC curves for four representative soils with the positions of the liquid limit and the plastic limit.

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Figure 9. Water content at a suction of 1500 kPa, as a function of wA.

certain water contents, and the values of wA, wL and wP more widely known index properties of soils: the Atterberg
are indicated in the graph. The SWCC is described using limits, the MBf value and the SWCC. Real soil samples
the Fredlund–Xing equation [17]. Different researchers with different origins and mineralogy were used, together
have investigated suction at the liquid and plastic limits with clean, commercially available limestone flour, brick
of different soils and have found different corresponding clay and bentonites, to determine whether the results are
values between 0.5 and 30 kPa [18], [19], [20]. comparable for different adsorption ranges. The following
conclusions may be drawn from the investigation:
The typical results presented in Figure 8 show that the
magnitude of the suction at the liquid limit of each • Linear trends are evident in the relationship between
specific soil depends on its Enslin-Neff water adsorption. the Atterberg limits and the Enslin-Neff water
This means that the value wA, which corresponds to the adsorption. This observation confirmed the results
maximum water content at zero suction, also controls published by Dieng [6]. By introducing a simplified
the suction at the liquid limit. equation (9), the classification of cohesive soil or
fines can be reasonably predicted from the Enslin-
The relationship between wA and the water content at Neff test. The Enslin-Neff test is faster, requires a
a suction of 1500 kPa is given in Figure 9. At least two very small sample, and is less subjective than the
different types of behaviour can be observed. The first Atterberg-limits test.
type belongs to the soil group R1, for which the wA
values are lower than 80%, and it corresponds to a water • Trends are indicated in the relationship between the
content at a suction of 1500 kPa of less than 7.5%. The MBf and the Enslin-Neff above values of wA > 60%.
second type belongs to the soils with wA values higher The strong influence of the nature of the exchange-
than 50% and a water content at a suction of 1500 kPa able cations on the MBf needs further investigation
of more than 7.5%. The amount of experimental data is in the direction of the MBf and the wA relationship.
too small to describe the relationship between the two However, the obtained results are promising, and
parameters, but the Enslin-Neff water adsorption could could be complemented by further investigations.
be estimated as the first point on the virgin SWCC.
• The wA was recognized as being probably the first
point on the “virgin” SWCC. Special connections
were recognized between the wA and the water
5 SUMMARY AND CONCLUSION content at the permanent wilting point. From this
point of view, the Enslin-Neff test provides new
An experimental program was conducted in the labora- possibilities for its use in the field of swelling-soil
tory with the aim of examining the physical meaning of classification methodology after additional testing
Enslin-Neff water adsorption (wA) in terms of some of the and certain modifications.

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 A. PETKOVS̆EK ET AL.: A LABORATORY CHARACTERIZATION OF SOILS AND CLAY-BEARING ROCKS USING THE ENSLIN-NEFF WATER-ADSORPTION TEST

The experimental results have confirmed the wide possi- surface areas and cation exchange capacities (Clay
bilities for the extended use of the Enslin-Neff method – organic studies XVIII). Clay and clay minerals,
in the laboratory for soil and rock mechanics and for 18, 203-212.
the testing of aggregates. It is especially suitable for soil [13] Çokça, E. (2002). Relationship between Methylene
classification and the preliminary estimation of the blue value, initial soil suction and swell percent of
possible volume changes of soils and clay-bearing rocks. Expansive Soils. Turkish Journal of Engineering and
As it is less subjective than the Atterberg-limits test and Environmental Sciences, 26, 521 – 529.
the MB titration method, it is a pity that the method has [14] Chiappone, A., Marello, S., Scavia, C. and Setti, M.
remained almost forgotten and was not introduced to (2004). Clay mineral characterization through the
soil mechanics laboratories earlier. methylene blue test: comparison with other experi-
mental techniques and application of the method.
Canadian Geotechnical Journal, 41, 1168-1178.
[15] Yukselen, Y., Kaya, A. (2008). Suitability of the
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