Geotextiles and Geomembranes xxx (xxxx) xxx–xxx

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Geotextiles and Geomembranes

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

A novel transient gravimetric monitoring technique implemented to GCL

osmotic suction control
A.S. Acikela, A. Bouazzab, W.P. Gatesc, R.M. Singhd, R.K. Rowee,∗
a
Formerly Monash University, Melbourne, Australia
b
Monash University, Melbourne, Australia
c
Deakin University, Burwood, Australia
d
Norwegian University of Science & Technology (NTNU), Trondheim, Norway
e
Queen's University, Kingston, Canada

A R T I C LE I N FO A B S T R A C T

Keywords: A modified osmotic suction control technique for monitoring apparent transient weight changes was successfully
Geosynthetic clay liner adapted to the wetting and drying paths of geosynthetic clay liners (GCLs). Reasonable control was possible,
Membrane behaviour enabling suction equilibrium to be achieved without disruption to the test. The results provide unique insight
Microstructure into the time-dependent changes in water retention properties and the semi-permeable membrane behaviour of
Osmotic method
the bentonite component in GCLs. The stages of suction equilibrium, related to the tri-modal pore structure of
Time dependency
GCLs and the point of capillary break, could also be monitored. While the osmotic method has been traditionally
used to control matric suction (up to 10 MPa) in soils, the overall results presented in this paper indicate that its
application for total suction control in GCLs is largely due to the membrane behaviour of their bentonite
component. Furthermore, because of capillary break between the GCL and the osmotic solution at the water
entry (or residual) suction value of a GCL, an upper limit of 2.8 MPa suction is recommended for the application
of the osmotic method to measure the water retention properties of GCLs.

1. Introduction thermocouple psychrometer, relative humidity sensor), or suction

Geosynthetic clay liners (GCLs) have been extensively used in waste
containment applications over the past two decades because of their
excellent sealing properties (Shackelford et al., 2000; Babu et al., 2001;
Bouazza, 2002; Gates et al., 2009; Scalia and Benson, 2010; Benson,
2013; Brachman et al., 2014; Liu et al., 2015; Touze-Foltz et al., 2016;
Bouazza et al., 2017; Rowe et al., 2017; Ozhan and Guler, 2018; Rowe,
2018; Scalia et al., 2018). GCLs are typically 6m wide rolls 20–30 m in
length and 5–10 mm thick. They are composed of sodium (mostly)
bentonite sandwiched between two geotextile layers through a needle
punching process which might include thermal treatment.
Understanding the water retention properties of GCLs is crucial to
better investigate clay-water interactions which govern their hydraulic
barrier performance (Bouazza et al., 2006; Siemens et al., 2012; Acikel,
2016; Acikel et al., 2018a, 2018b; Leong et al., 2018; Rowe, 2018,
2020; Ghavam-Nasiri et al., 2019; Tincopa et al., 2020). The water
retention of GCLs has been investigated using direct (tensiometer) and
indirect suction measurements (filter paper, chilled mirror,
control techniques (osmotic, vapour equilibrium, pressure plate and
pressure membrane extractor) since the early 90s (Daniel et al., 1993;
Barroso, 2005; Bouazza et al., 2006; Southen and Rowe, 2007; Abuel-
Naga and Bouazza, 2010; Acikel et al., 2011, 2015; 2018a, 2018b;
Beddoe et al., 2011; Bannour et al., 2014; Seiphoori et al., 2016; Lu
et al., 2017; Carnero-Guzman et al., 2019; Yesiller et al., 2019).
The unsaturated behaviour of GCLs is highly relevant for assessing
their performance as components in modern composite liners, but to
date many obstacles have limited this understanding. First, no single
control technique can cover – within the accuracy and applicable limits
of the method – the entire suction range of a typical water retention
curve (WRC) of a GCL (Abuel-Naga and Bouazza, 2010; Beddoe et al.,
2011; Acikel et al., 2015; Leong et al., 2018). Secondly, the required
measurement times for attaining suction equilibrium (or even steady
state) makes obtaining unsaturated behaviour data on GCLs quite
complicated (Acikel et al., 2018a). Finally a significant challenge lies in
the difficulty of maintaining capillary connection between the GCL
specimens and the transfer medium (osmotic, filter paper, pressure

∗
Corresponding author.
E-mail addresses: asliacikel@gmail.com (A.S. Acikel), malek.bouazza@monash.edu (A. Bouazza), will.gates@deakin.edu.au (W.P. Gates),
rao.m.singh@ntnu.no (R.M. Singh), kerry.rowe@queensu.ca (R.K. Rowe).

https://doi.org/10.1016/j.geotexmem.2020.05.002
Received 15 February 2020; Received in revised form 30 April 2020; Accepted 4 May 2020
0266-1144/ © 2020 Elsevier Ltd. All rights reserved.

Please cite this article as: A.S. Acikel, et al., Geotextiles and Geomembranes, https://doi.org/10.1016/j.geotexmem.2020.05.002
A.S. Acikel, et al.
Fig. 1. Tri-modal pore structure of GCL (Modified from Acikel et al. (2018a)).
plate, pressure membrane extractor) during measurements. In addition,
a failure in establishing and maintaining the capillary contacts had
serious repercussions on hydration of GCLs from subgrade (Acikel et al.,
2015, 2018b).
The GCL tri-modal pore structure has been considered in few studies
(Joe et al., 2006; Acikel et al., 2018a,b). Jo et al. (2006) defined the tri-
modal pore size as inter-granular, inter-particle, and interlayer pores;
while, Acikel et al. (2018a,b) defined it as macropores (geotextile
pores), mesopores (bentonite inter-aggregate pores) and micropores
(intra-aggregate, inter-particle, intra-particle and interlayer pores)
(Fig. 1). In addition, the bentonite component of GCL itself was also
widely accepted to have a bi-modal pore structre with its inter- and
intra-aggregate pores (Gens and Alonso, 1992; Alonso et al., 1999;
Sanchez et al., 2006; Delage, 2007; Villar and Lloret, 2008; Romero
et al., 2011; Navarro et al., 2015; Cui, 2017).
The time-dependent unsaturated behaviour during water uptake (or
release) by the bentonite component of GCLs results in difficulties in the
measurement or control of suction in GCLs (Delage et al., 2006; Schanz
et al., 2010). Recently, Acikel et al. (2018a) reported that the measured
suction values of GCLs were dependent on time (i.e., time after change
in water content) and duration of measurement. GCLs have different
time-dependent suction change behaviours linked to wetting or drying
paths, within specific water content ranges that are influenced by either
the bentonite component (meso and micropores) or the geotextile
component (macropores) (Acikel et al., 2015, 2018a; 2020). For prac-
tical applications, the quasi-equilibrium state of the bentonite (Schanz
et al., 2010) component and its overall impact on GCLs should be
considered in terms of accuracy and repeatability of wetting and drying
WRC paths when implementing numerical analyses (Acikel et al.,
2018a).
This paper introduces a novel application of the osmotic method for
monitoring hydration and dehydration under suction control to provide
further qualitative insight into time-dependent hydration and dehy-
dration behaviour of GCLs. The technique is based on transient weight
measurements of GCLs on both wetting and drying paths within a
suction range of 100 to 3900 kPa. This paper examines three key clay-
water interaction aspects of the GCLs, which are: (1) time-dependent
changes in retention properties, (2) semi-permeable membrane beha-
viour of the bentonite component and (3) whether the osmotic method
controls matric suction or total suction when applied to GCLs.
1.1. Osmotic technique
Aqueous polyethylene glycol (PEG) solutions and semi-permeable
membranes are typically used as a matric suction control method.
Theoretically, a semi-permeable membrane is permeable to water (and
2
Geotextiles and Geomembranes xxx (xxxx) xxx–xxx
dissolved ions present in pore water) but impermeable to soil particles
and polyethylene glycol (PEG) molecules, which have molecular weight
(MW) greater than the molecular weight cut off (MWCO) value of the
membrane (Zur, 1966). MWCO can be described as the lowest mole-
cular weight of a PEG solute, of which ≥90% can be excluded by the
membrane. The osmotic method requires capillary contact through the
semi-permeable membrane between the specimen and a solution of a
high osmotic electrolyte of PEG to obtain an accurate measurement of
matric suction. After establishing capillary contact, the transfer of water
and soil ions between the specimen and the PEG solution will continue
until the matric suction of the specimen becomes equal to the osmotic
suction of the solution created by the PEG.
Polyethylene glycol (PEG) is a polyether compound which has a
generic formula of H-[O–CH2–CH2]n-OH where n is an integer re-
presenting the number of repeating polymer units, and thus the length
of the alkyl-ether chain. PEG molecules with large n have greater unit
masses (g/mol) or molecular weights (MW). PEGs are classified based
on their unit masses, e.g., PEG 1000 indicates that the molecular weight
is 1000 g/mol. Delage and Cui (2008) stated that PEG 6000 and 20,000
are the most commonly used PEGs in geotechnical engineering and
presented an empirical correlation (Eq. 1) relating PEG concentration,
c, and the resulting osmotic suction, s:
s = 11 × c 2 (1)
where c is the mass of PEG per mass of water.
Tripathy and Rees (2013) prepared PEG solutions within an osmotic
suction range between 0.09 and 12.2 MPa using PEG 1,500, 4,000,
6000 and 20,000. They measured the suction values of the solutions
with a chilled mirror technique and found good agreement between the
measured suction values and the results reported in the literature.
The semi-permeable membranes have to retain the lower limit of
the molecular weight of the PEG solute. MWCO is a characteristic
parameter of dialysis membranes. Table 1 lists the molecular weight
(MW) of some PEGs and corresponding MWCO values of dialysis
Table 1
Molecular weight (MW) of the common polyethylene glycols
and molecular weight cut off (MWCO) values of the re-
commended semi-permeable membranes (Delage and Cui,
2008).
MW of PEG (g/mol) MWCO (g/mol)
1500 1000
4000 2000
6000 3500
20,000 12,000–14,000
A.S. Acikel, et al. Geotextiles and Geomembranes xxx (xxxx) xxx–xxx

membranes recommended by Delage and Cui (2008).
The osmotic method has advantages over other suction control
methods as the test can apply realistic pressure conditions and can
reach high suction values without using high air pressures as used in
axis-translation method. However, the reliability of the semi-permeable
membranes has been questioned (Williams and Shaykewich, 1969).
Tarantino and Mongiovi (2000) observed that all membranes had a
threshold suction value, and beyond this value, solute PEG molecules
were no longer retained by the semi-permeable membrane and passed
into the sample. Tripathy et al. (2011) applied 0.44 and 7.04 MPa
suctions on the semi-permeable membranes with MWCO 14,000 and
3500 respectively. They reported that higher suction values (i.e.
7.04 MPa) increased the pore sizes of the membrane and could cause
penetration of the PEG molecules in the soil specimen through the
membrane.
Another concern of the longer term measurement or control tech-
niques has been microbial growth (Leong et al., 2002; Barroso et al.,
2006; Acikel et al., 2015). Tadza et al. (2017) successfully conducted
osmotic tests under short length ultraviolet germicidal irradiation
(UVGI) to avoid microbial growth.
2. Material and methodology
2.1. Material
Three commercially available needle-punched GCLs were used in
this study. Their engineering and material properties of the GCLs used
in the current study are shown in Table 2. GCL1 (Elcoseal X2000) and
GCL2 (Elcoseal X1000) consisted of powdered sodium bentonite from
the same source, whereas GCL3 (Bentomat ST) had granular based so-
dium bentonite from a different source. GCL1 and GCL2 were thermally
treated, whereas GCL3 was not. GCL1 had a scrim-reinforced woven
carrier and a nonwoven cover geotextile, whereas GCL2 and GCL3 had
a woven carrier geotextile and a nonwoven cover geotextile.
2.2. Experimental setup
The experimental setup allowed transient gravimetric monitoring of
the GCL specimen suspended in PEG solutions of known osmotic suc-
tion. The traditional osmotic method was modified to enable transient
gravity monitoring of apparent mass changes of the specimen during
the suction control tests. The modified method allowed close mon-
itoring of the suction quasi-equilibrium and true equilibrium stages
between the PEG solution and the GCL specimen. Moreover, the system
allowed real-time observation of hydration and dehydration occurring
within the GCLs. A schematic configuration of the osmotic method
setup is shown in Fig. 2(a). Fig. 2(b) and (c) show a GCL specimen in the
PEG solution at the beginning and the end of a drying path osmotic test,
respectively.
The setup consisted of a magnetic stirrer, a glass container with a
lid, a stirrer bar, dialysis membrane, membrane closures, PEG solution,
distilled water, a monofilament line, three thermocouples, a tempera-
ture logger, a 0.0001 g sensitivity digital scale, a plexiglass housing,
and a black foam rubber platform (Fig. 2(a)). The plexiglass housing
was used to minimize air disturbance as well as the effects of changes in
temperature or relative humidity on the water re-distribution process
during the tests. The plexiglass housing was placed on a black foam
rubber to absorb and dampen any possible vibrations. The digital scale
was set on the upper shelf of the housing. A hole in the shelf was
aligned to the centre of the hanger beneath the digital scale to allow
continuous monitoring of the GCL weight.
The glass container with the PEG solution was placed on a hotplate/
magnetic stirrer located on a lower shelf. The glass container and the
magnetic stirrer were aligned with the centres of the holes in the upper
shelf and the small hole in the centre of the lid of the glass container. A
thermocouple connected to the magnetic stirrer was immersed into the
solution through the monofilament line through another small hole
close to the edge of the lid. A cork was used to position the thermo-
couple in the solution and inhibited evaporation through the hole. The
hotplate/magnetic stirrer kept the solution at the set room temperature
of 22 ± 2 °C.
Two K-type thermocouples were used to monitor possible tem-
perature fluctuations close to the scale and the glass container. One of
the thermocouples was placed at the bottom of the digital scale and the
other one on the side of the glass container. The thermocouples were
connected to a computer through a temperature logger for data ac-
quisition. The digital scale was also connected to the computer to log
the mass changes (transient gravimetry) of the specimen submerged in
the PEG solution.
The GCL specimen in the dialysis membrane was hung from the

Table 2
Engineering and material characteristic of GCLs (Acikel et al., 2018a,b).
Mass per unit area (g/mb) GCL1 GCL2 GCL3

GCL Measured 4885 5266 4698

MARVd (ASTM-5993 2014) 4350 4380 4000
Bentonite Calculated 4159 4745 4273
MARVd(ASTM-5993 2014) 3700 4000 3600
Carrier geotextile Measured 438 135 126
Cover geotextile Measured 288 386 299
Saturation (Reference) gravimetric water contents (GWCsat) under 1 kPa vertical static loading 205% 202% 206%
Bentonite Particle type powdered powdered granular
Cation Exchange Capacity (CEC) (cmolc/kg) 76 79 92
Smectite (XRD test results) a 80% 79% 82%
Initial (off-roll) gravimetric water content (ASTM-D2216 2010) 10% 11% 12%
Liquid limit (ASTM-D4318, 2000) 755% 772% 370%
Plastic limit (ASTM-D4318, 2000) 46% 46% 36%
Swell Index (ml/2g) (ASTM-D5890, 2011) 22 22 22
Hydraulic conductivity b (m/s) (ASTM-D5887 2009) 3 × 10−11 3 × 10−11 5 × 10−11
Structure Configuration (Carrier/Cover) SRW/NW W/NW W/NW
Bonding NP NP NP
Peel Strength (N/m) (ASTM -D6496, 2009) c 1855 750 610
Thermally treated yes yes no

a
XRD tests conducted at CSIRO Land and Water, Mineralogical Services, Adelaide laboratory.
b
Max values as provided by the manufacturers.
c
Obtained from manufacturers.
d
MARV: minimum average roll value (from producer), SRW: scrim-reinforced woven, W: woven, NW: nonwoven, NP: needle-punched.

3
A.S. Acikel, et al.
Fig. 2. (a) Schematic configuration of the osmotic test apparatus, (b) The osmotic test specimen at the beginning, (c) at end of the drying test.
bottom hanger of the digital scale and into the PEG solution through the
hole in the centre of the lid. Weighted membrane closure clips attached
to the ends of the membrane (Fig. 2) ensured that the specimen did not
allow the PEG solution in and that it remained fully submerged within
the solution.
PEG 20,000 and standard regenerated cellulose (RC) semi-perme-
able membranes of 12–14,000 MWCO (Spectra/Por®4) were used in the
present investigation. The dry membrane contained glycerine as a hu-
mectant and, therefore, soaking and rinsing in water before use was
required to eliminate the possibility of glycerine impacting the osmotic
potential of the excess water. The tube opening of the membrane had a
spherical-equivalent diameter of 29 mm.
A data acquisition software was developed to log the temperature
and apparent mass change data simultaneously. The software program
permitted changes to the data logging frequency any time during the
test without impacting the dataset. Two temperature data loggers in
conjunction with the K-type thermocouples were used to record tem-
perature changes from the digital scales and the glass containers.
4
Geotextiles and Geomembranes xxx (xxxx) xxx–xxx
2.3. Methodology
The osmotic method consisted of three stages; stage 1 was devoted
to preparation, stage 2 to testing, and stage 3 to validation of the final
suction of the specimen using chilled-mirror measurements. The pre-
paration stage included preparation of the specimen, membrane, PEG
solution and the test preparations. The testing stage related to mon-
itoring and finalizing the osmotic test and chilled mirror measurements.
Suction measurements using the chilled-mirror method were performed
to validate the final attained suction values of the specimens after os-
motic tests. A dew point potentiometer, WP4C, was used for the chilled-
mirror measurements.
Different procedures were applied for the preparation of the speci-
mens for drying and wetting path tests, but the same test method was
used for both paths. The wetting path specimens were cut from air-
dried GCL samples to predetermined sizes, and silicon glue was smeared
around their periphery to avoid bentonite loss. The dimensions of the
specimens were selected considering the diameter of the open dialysis
tube and the expected volume changes during wetting/drying paths.
A.S. Acikel, et al.
Table 3
Determination of the width of the wetting path specimens by considering the free hydration test results and the perimeter of the membrane.
GCL Maximum strain at 90% of saturationa Air dried condition
Δt/t Δw/w a
tmax (mm) w (mm)
a B C d
GCL1 0.22 0.02 9.4 29
GCL2 0.34 0.09 7.0 29
GCL3 0.34 0.04 8.3 29
t: thickness, w:width.
a
Values obtained from the free hydration tests.
The thickness of the silicon edges was also considered during the wet-
ting path specimen size calculations.
The maximum change of the thickness and width of the GCL spe-
cimen at 90% reference gravimetric water contents (wref) as well as the
maximum thickness values obtained from free hydration tests were
used to estimate the sizes of the specimen. The optimal size of the
wetting path specimens was determined as 29 ± 2 mm in width and
58 ± 2 mm in length (two times the width) (Table 3). The wref values
of GCLs were defined as the maximum gravimetric water content that
can be achieved under specific loading conditions (Rayhani et al., 2011;
Singh and Bouazza, 2013; Ali et al., 2016; Rouf et al., 2016; Acikel
et al., 2018b).
The initial gravimetric water content of 90% of wref (Table 2) was
chosen as representative of the maximum hydration of the virgin wet-
ting before starting the virgin drying path to avoid the possible and
irreversible bentonite loss that is known to occur above ≈ 100% of wref
(Acikel et al., 2018a, 2018b). Thus, the values of the 90% wref were used
for the estimations of any volume change occurring in the test spe-
cimen.
The initially air-dried 153 mm × 115 mm specimens were hydrated
with distilled water to ~90% of wref (Table 2). Then the specimens were
conditioned for two weeks in sealed containers under 1 kPa sitting load
in a 22 ± 1 °C constant temperature room to achieve a uniform water
content distribution after hydration (Vangpaisal and Bouazza, 2004; Ali
et al., 2016; Rouf et al., 2016). At the end of the pre-conditioning time,
the specimens were cut to drying path specimen sizes of 32 ± 2 mm in
width by 64 ± 2 mm in length.
The PEG solutions were prepared based on the empirical Eq. [1]
suggested by Delage and Cui (2008). The solutions were stirred using
magnetic stirrers until the PEG was dissolved entirely and then were
continuously stirred to keep them homogenous. A thermocouple was
inserted in the solution, through the hole in the lid of the container, to
monitor temperature continuously. Then, the stirrer/hotplate was set to
22 °C.
The preparation procedure was conducted as rapidly as possible to
minimize exposure of the specimen to air. The semi-permeable mem-
brane tube was cut to a length of ~150 mm. After a minimum 1-h
submersion in distilled water, the membrane tube was opened so that
the GCL specimen could be inserted as quickly as possible while both
the sample and the tube were submerged in distilled water to minimize
the presence of air in the system. The submersion also enabled quick
contact with the PEG solution during the tests. During sample insertion,
any entrapped air and excess distilled water were also removed through
both ends of the tube, which were then sealed using membrane clips. A
small amount of excess distilled water (generally less than 1 mL) in-
evitably remained in the tube. Finishing the process quickly was es-
sential for the wetting path to avoid excessive initial hydration of the
specimen before commencing the osmotic tests.
A monofilament line then was tied to the membrane closers, and the
specimen was placed in the PEG solution. The line was fed through the
hole in the lid of the glass container, the lid was closed, and the other
end of the line was fastened to the bottom of the digital scale so that the
5
Geotextiles and Geomembranes xxx (xxxx) xxx–xxx
90% wref tsilicon (mm) Perimeter of specimen (mm)
tmax (mm) w (mm)
e = c (1 + a) f = d (1 + b) g 2 (e + f + g)
11.5 29.6 4 90
9.4 31.6 4 90
11.1 30.0 4 90
specimen was suspended while immersed within the PEG solution. Care
was taken to ensure that the specimen did not touch the sidewalls of the
container.
At the end of the test, the monofilament was cut, and the membrane
was taken out of the PEG solution. One of the membrane closure clips
was removed, and the GCL specimen was then extracted from the
membrane using tweezers. Any contact of the GCL specimen with PEG
solution or deformation of the specimen with the tweezers was avoided
during this process. The gravimetric water content of one half of the
GCL specimen was directly measured after the osmotic test. The other
half of the specimen was carefully cut to fit into a WP4C specimen
container before a chilled-mirror test was run to measure the specimen
suction.
3. Results and discussion
3.1. Transient gravimetric monitoring results
The transient gravimetric monitoring method is intended to give
insight into the hydration or dehydration states of the specimen, and
whether or not the specimen had attained equilibrium to a particular
osmotic potential at any specific time. The actual hydration/de-hy-
dration paths of the specimens were monitored without disrupting the
paths.
The weight changes recorded were not a direct measure of water
uptake or loss because the GCL specimen was suspended in a PEG so-
lution that was agitated with a magnetic stirrer. Instead, the weight
change measurements correlate with water uptake or loss and are af-
fected by the centrifugal force created by the stirrer and the buoyancy
of the PEG solution. Thus, while the measured data were associated
with the weight change in the specimen due to water uptake or loss, the
data was an indirect measure of weight, termed here the apparent
weight. Thus, the logged data was the change in the tensile force
transmitted through the monofilament line which is equal to the change
in the resultant force of the specimen weight, the centrifugal force
created by the stirrer, and the buoyancy due to the PEG solution.
Figs. 3 and 5 to 9 show selected transient gravimetric monitoring
data of different osmotic suction control tests to facilitate discussion of
the various stages associated with either drying or wetting paths.
Figs. 3, 5 and 6 show monitoring data from the drying path tests, while
Figs. 7–9 show those of the wetting path tests.
Transient gravimetric monitoring data show sharp initial increase
and/or decrease patterns within the first hours of the test. These in-
crease/decrease patterns indicate that the excess water in the mem-
brane was distributed between the specimen and the PEG solution. The
process of excess water distribution was vital to establish and maintain
proper capillary connections. It is to be noted that proper capillary
connections between the specimen and PEG solution are essential for
osmotic method.
Fig. 3 was obtained from GCL1 during a drying test to the target
suction value of 200 kPa. The apparent weight change of GCL1 stabi-
lized after approximately 2.5 days, but then increased slightly after day
A.S. Acikel, et al.
Fig. 3. Apparent weight and temperature change versus time for the 200 kPa suction drying path test of GCL1.
four. The simultaneously logged temperature monitoring data show
that temperature fluctuations were small and did not have a pattern to
indicate an impact at the changes in transient weight. The probable
causes of this increase are discussed later in this section. The test was
stopped when the increase in weight change became steady; however,
this increase was not significant.
After the drying path osmotic suction control test was completed
(under 200 kPa suction), a part of the GCL specimen was placed in the
chilled-mirror test container and kept sealed for an hour and then
placed in the chamber of the chilled-mirror test device (WP4C) for
suction measurement. The total suction result obtained by the WP4C
was 230 kPa. After completion of the chilled-mirror test, the specimen
was kept sealed in the chilled-mirror test container, and the suction
measurement was repeated one week later. The one-week suction result
was 190 kPa. The time-dependent drop in the suction values obtained
by the measurements taken 1 h and one week after the osmotic test was
similar to the time-dependent behaviour reported by Acikel et al.
(2018a) where, for a suction range < 2800 kPa, the total suction
Fig. 4. Fourier transform infrared (FTIR) spectrometry results for the GCL1 specimen after (a) 200 kPa wetting path, (b) 2000 kPa drying path (short), and (c)
2000 kPa drying path (long) osmotic tests.
6
Geotextiles and Geomembranes xxx (xxxx) xxx–xxx
decreased with time at a constant gravimetric water content.
Note that the chilled-mirror test device WP4C has a reported ac-
curacy of ± 50 kPa for the suction range of 0–5000 kPa (Decagon
Devices Inc, 2016), and that the aforementioned changes in total suc-
tion are within that error. A back-calculation was performed on the PEG
solution to estimate the final suction value after suction equilibrium
with the GCL. The effect of exchanged water with the GCL specimen
and excess water in the membrane on the PEG concentration was taken
into account for the calculation. The final suction value of the PEG
solution was 197 kPa. Therefore, both suction results obtained by WP4C
were comparable with the final suction value of the PEG solution,
considering the reported accuracy limit of ± 50 kPa of the device. The
results indicate that the specimen reached suction equilibrium with the
PEG solution when the test was completed.
The impact of gravity on water content distribution between the two
pieces of specimen was very small (~0.28 kPa) compared to the applied
suction values (100–3900 kPa). Thus, this impact was deemed to be
negligible. In addition, WP4C device had no sensitivity to measure a
A.S. Acikel, et al.
Fig. 5. wt and temperature change versus time for the 200 kPa drying path test
of GCL2.
Fig. 6. GCL1 2000 kPa drying path duplicated tests (a) weight change (b) PEG
solution temperature monitoring. Black color shows the short test and grey
color shows the long test data.
Fig. 7. wt and temperature change versus time for the 200 kPa wetting path test
of GCL1.
suction difference of 0.28 kPa.
Another concern was whether any PEG may have passed through
the dialysis membrane (e.g., via the clamped ends of the tube, or due to
membrane failure) and then interacted with the bentonite within the
GCL. To test this hypothesis, a portion of the GCL specimen was ana-
lysed using Fourier transform infrared (FTIR) spectrometry after the
osmotic test and the subsequent WP4C suction measurements. The
7
Geotextiles and Geomembranes xxx (xxxx) xxx–xxx
expected absorption bands for PEG molecules range between 2800 and
3000 cm−1, associated with aliphatic C–H stretching, as well as bands
between 1100 and 1400 cm−1 associated with C–H and O–H bending
and C–O(H) stretching (Shameli et al., 2012). If significant PEG leaked
through the membrane and into the specimen, the PEG would interact
strongly with the bentonite component. However, no evidence of these
bands was detected in the bentonite component of the GCL specimen
collected subsequent to the tests (Fig. 4), indicating that the membrane
remained intact.
The weight and temperature changes related to the drying path
osmotic test of GCL2 in a 200 kPa PEG solution are shown in Fig. 5. The
figure indicates that the weight change of the specimen stabilized after
the first day, after which the system remained in equilibrium until the
test was terminated before the third day. One hour after the termination
of the osmotic test, the WP4C measurement gave a suction of 220 kPa.
Considering the ± 50 kPa accuracy of the WP4C device, the result was
within the range of the calculated final suction value of the PEG solu-
tion, 196 kPa.
Duplicated tests were performed at 2000 kPa on the drying path of
GCL1 using two osmotic setups simultaneously, and the tests were
competed at different times. Fig. 6 shows the weight change and PEG
solution temperature of the duplicates. The duplicates followed very
similar paths for the first 3.8 days. The weight decreased for the first
half-day (point I), then increased to reach a peak followed by another
dip (point II) at approximately three and a half days after the tests
started. The weight of the duplicates started to increase again after 3.6
days, indicating membrane failure. One of the tests (short test) was
stopped at the onset of the weight increase. The other (long) test was
allowed to continue for 10 days in total. The linear increase in weight
after approximately 5 days after the test started (point III) continued
until the long test was stopped to compare the impact of linear increase
behaviour. Points I and II are interpreted as indicating the suction
equilibrium of different pore sizes in the multiporous structure of the
GCLs. Point I likely relates to the largest pores of the geotextile and
Point II probably indicates the quasi-equilibrium stage between ben-
tonite macro and micro pores (Acikel et al., 2018a). Such two-step
equilibrium was not observed in the tests under 200 kPa suction control
(Figs. 2 and 4), since the micro pores in that suction range were satu-
rated, and the bentonite gel was formed (this is further discussed sub-
sequently in this section).
The total suction results (Table 4) of the short test specimen 1 h and
one week after the osmotic test were 1950 kPa and 1975 kPa, respec-
tively. These results compare favourably with the back-calculated final
suction value of the PEG solution (1951 kPa). Therefore, the GCL
sample in the short test reached suction equilibrium with the PEG so-
lution. Moreover, measured suction values were within WP4C error
range ( ± 50 kPa).
The total suction values (Table 4) at 1 h and one week for the GCL
specimen used in the long test were 2080 kPa and 1245 kPa, respec-
tively. There was a suction difference of 157 kPa between the specimen
and the PEG solution (2080 kPa and 1923 kPa, respectively) 1 h after
the test, but a greater difference (678 kPa) in the one-week suction
result.
To investigate if the difference in suction values as indicated in the
osmotic suction of the GCL specimen resulted from possible PEG in-
trusion due to membrane failure, FTIR spectra of the specimen were
collected. According to the FTIR test results (Fig. 4b and c), no clear
evidence of PEG intrusion into the specimen was detected. Therefore,
some other mechanisms, such as deterioration of the PEG and loss of
osmotic suction, may have impacted the results.
As previously discussed, Figs. 3 and 5 show drying path results
under 200 kPa suction control of GCL1 and GCL2, respectively. Final
calculated suction values for both PEG solutions were 197 and 196 kPa,
and the final water contents of the GCL1 and GCL2 were 129% and
131%, respectively. The reference gravimetric water contents (wref) of
the GCLs were ~200% (Table 2). In this case, both final water contents
A.S. Acikel, et al. Geotextiles and Geomembranes xxx (xxxx) xxx–xxx

Fig. 8. wt and temperature change versus time for the 300 kPa wetting path test of GCL2.

were above 50% of wref. The ranges of initial and final water contents Table 4
correspond to the unconfined inter-particle or excess surface water of Suction values of the PEG solution (initial and final) and GCL1 specimens of the
the bentonite (Acikel et al., 2018a, 2018b). Due to drying within the duplicated drying path tests at 2000 kPa. The suction values of the specimens
macro-pore water ranges of bentonite, the quasi-equilibrium stage as were measured by WP4C 1 h and one week after the OT (osmotic test).
observed for the test at a suction value of 2000 kPa (Fig. 6) was not Test GCL gravimetric water Osmotic suction of the Total suction of the GCL
observed in these two tests (Figs. 3 and 5). content PEG solution (kPa) specimen (kPa)
Fig. 7 shows transient gravimetry monitoring data of the wetting
Initial Final Initial Finala 1 h after 1 week
path osmotic test for GCL1 under 200 kPa suction control. The sample
OT after OT
weight stabilized 5.5 h after the test started and stayed relatively con-
stant up to approximately day two. Then, the weight increased linearly Short 185 ± 5% 36% 2000 1951 1950 1975
until the test was stopped at day ten due to concerns about the mem- Long 185 ± 5% 41% 2000 1923 2080 1245
brane integrity. a
Calculated value.
The WP4C results 1 h and one week after the osmotic test were
480 kPa and 440 kPa, respectively, confirming that the osmotic test did
under 300 kPa suction control wetting path test. The specimen had a
not reach suction equilibrium when the test was stopped. One possible
break-point in the apparent weight change rate after one day (point I),
explanation for this behaviour is that the large pores would have filled
and the rate of weight increase slowed after day eight (point II). Similar
up with liquid quickly, but the finer pores would have filled up more
to the results shown in Fig. 7, the break-point (point I) probably results
slowly so that water uptake occurred over overlapping times for both
from formation of an unstable state of the GCL when the swelling
pore size ranges. Water filled the finer pores later, but once accessed,
pressure of the bentonite reached the entanglement limit of needle-
more and more of them become filled. This process resulted in the in-
punched fibres that delayed the change in GCL thickness. After point I,
itial levelling off and then increase in water uptake.
the extension of the needle-punched fibres (Gates et al., 2018) allowed
The non-woven needle punched textile fibres of the GCL may also
both bentonite swelling and further water uptake. As such, the water
have played a role in the water uptake pattern (Fig. 7). Initially, the
content at point I probably indicates the volume of macro-pores (due to
fibres may have slowed the water uptake, because they are anchored to
the skeleton of the geotextiles fibres) within the tri-modal pore struc-
the base geotextile component of the GCL, and anchoring can be very
ture of GCLs (Acikel et al., 2018a, 2018b). After full extension of the
strong if thermal treatment has been conducted on the GCL, giving the
geotextile fibres at point I, point II might indicate the stage between
appearance of equilibrium. Swelling bentonite will exert a pulling force
quasi and true equilibrium of suction.
on the needle-punched fibres, and the weaker the anchorage and de-
The WP4C total suction measurements of the GCL2 specimen which
formation of the fibres, the greater the water uptake (Gates et al.,
were taken 1 h and one week after the 300 kPa wetting path osmotic
2018). Similar hydration patterns have also been observed in free hy-
test were 550 and 340 kPa respectively. While the first WP4C mea-
dration tests (Acikel, 2016; Acikel et al., 2018b).
surement (550 kPa) overestimated the suction result expected if the
Fig. 8 shows transient gravimetry changes of a GCL2 specimen

Fig. 9. wt and temperature change versus time for the 300 kPa wetting path test of GCL2.

8
A.S. Acikel, et al.
sample approached a steady state with the osmotic suction of the PEG,
the second test result (340 kPa) was comparable with the final suction
value (300 kPa) within the accuracy limits of the device. The WP4C
results also confirmed the transient gravimetric monitoring results for
the GCL: when the test was terminated, the GCL specimen was not at
equilibrium.
Within the 200–300 kPa suction range more than ten days was re-
quired to achieve suction equilibrium (Figs. 7 and 8). Alternatively, to
speed up the approach to equilibrium at lower suction values in the
wetting path, the specimen can be initially hydrated to a target water
content. However, the initial water content needs to correspond to a
higher suction than the target suction to avoid wetting-drying hyster-
esis.
Fig. 9 shows the weight and temperature changes during the GCL3
(non-thermally treated) wetting path osmotic test under 800 kPa suc-
tion control. The figure indicates three clear stages of water uptake.
These stages might be interpreted as:
(1) Three progressive stages of fibre anchorage failures (e.g., disen-
tanglement, stretching and breaking) to the carrier geotextile due to
swelling pressure of bentonite; or,
(2) Three steady states related to different pores sizes within the triple-
porous structure (Fig. 1) of the GCL: macro- (geotextile), meso-
(inter-aggregate), micro- (intra-aggregate and smaller) pores
(Acikel et al., 2018b); or,
(3) A combination of the processes outlined in (1) and (2).
WP4C measurements performed 1 h and one week after the osmotic
test were 1190 and 790 kPa respectively. Similar to the WP4C total
suction measurements after the 300 kPa wetting specimen of the GCL2
(Fig. 8), the first measurement was higher than the target suction value
of the suction control test, while the second test was highly comparable
with the final calculated value of the solution, 801 kPa. The results
likely indicate that the specimen was at a steady state near equilibrium
when the test was terminated.
However, WP4C suction measurements on the drying path de-
termined from the osmotic method specimens 1 h after the tests were
highly comparable with the target suction with approximately 3% dif-
ference. A drop in the suction values of the one-week measurement then
occurred, similar to the results from the wetting path as well as previous
chilled mirror results (Acikel et al., 2018a). As dsicussed by Acikel et al.
(2018a), when the system reachs a steady state at a constant water
content on a wetting path within the lower suction range (< 2800 kPa),
the measured suction continues to drop with time due to a re-dis-
tribution of water within the microstructure of the bentonite compo-
nent. Eventually a true equilibrium condition is established.
Some possible mechanisms that may explain the linear increases in
the gravimetric monitoring data following stabilization points are:
1 The suction equilibrium at the microstructural level was not at-
tained, because the bentonite continued to hydrate and swell.
2 Changing suction (dis-equilibrium) due to the transfer of excess
cations from GCL to the PEG solutions.
3 Loss of osmotic suction in the PEG solution due to deterioration of
the PEG.
4 The buoyancy in the PEG solution changes with time due to both the
volume change of the specimen and also the density change of the
PEG solution after the water content changes of the GCL specimen.
5 Water uptake as a result of progressive failure in needle-punched
fibre anchorage to the carrier geotextile due to bentonite swelling
pressure.
The observed linear increase in weight may have been due to any
one of the aforementioned mechanisms, or a combination of two or
more. However, further research is needed to identify which cause
might be significant. After the steady state was reached with the macro-
9
Geotextiles and Geomembranes xxx (xxxx) xxx–xxx
structure of the GCL (pore sizes due to the geotextile pores or bentonite
macro-pores) and the PEG solution, the suction of the specimen started
to change over time due to time-dependent behaviour as discussed by
Acikel et al. (2018a). However, since the osmotic method is a suction
control technique and not a measurement technique, the PEG solution
tends to keep the specimen at a specific suction value when the time-
dependent changes are happening in the specimen.
3.2. Applicability of the osmotic method to GCLs
Capillary connections between the specimen and PEG solution are
necessary for the osmotic technique on GCL suction control to be valid.
The highest applied suction in the wetting path was initially 3900 kPa
(GCL3), and when the test was terminated, the suction value of the PEG
solution was 3872 kPa. The WP4C measurement of the GCL specimen
after this test gave a suction value of 5940 kPa. This difference is ex-
plained as being a result of the specimen hydrating only from the excess
water entrapped within the membrane when the test started. As a result
of the difference in osmotic suction between the PEG and GCL sample
capillary connectivity between both sides of the membrane failed once
the excess water was taken up by the specimen. On the drying path
osmotic tests for the same high suction range (3000–3900 kPa), the
suction values of the GCL specimens measured by WP4C after the os-
motic tests were terminated were lower than the final osmotic suction
of the PEG solution. These results also support the fact that capillary
failure probably happened prior to the establishment of suction equi-
librium between the PEG solution and the specimen. Therefore, tran-
sient gravimetry monitoring was unsuccessful at the highest applied
suction values (3000–3900 kPa), especially on the wetting paths of the
GCLs and the upper suction limit for the use of the osmotic method
depends on the residual suction value of the specimen. This suction
range lies within or close to the WRC residual zone of the GCLs (Acikel
et al., 2018a, 2018b), which indicates that capillary connection be-
tween GCLs and the PEG solution could not be maintained properly
during the osmotic test for suction values higher than 3000 kPa. The
suction range is also comparable to the suction value of saturated
bentonite (4 layer water) which was reported to be around 2800 kPa
(Saiyouri et al., 2004) for Na-bentonite (MX-80). According to the
transient gravimetry and suction results, the use of the osmotic suction
control method is not recommended for suction values > 2800 kPa.
3.2.1. Does osmotic method control GCL matric suction or total suction?
Traditionally, the osmotic technique has been used as a matric
suction control technique, since a semi-permeable membrane is
permeable to water and soluble salts present in the soil, but is not
permeable to PEG molecules. However, in the case of GCL, the bento-
nite component itself will act as a semi-permeable membrane, and
therefore, will hold some soluble salts. Considering the working prin-
ciples of the osmotic technique and semi-permeable membrane beha-
viour of bentonite, the osmotic technique, when applied to bentonites
or GCLs, is hypothesized herein to be a total suction, rather than a
matric suction, control technique.
The bentonite component of GCLs is dominated by sodium cations
(Na+), which migrate from the interlayer spaces of the smectite if ex-
changed by other cations (Herbert and Moog, 1999; Likos et al., 2010;
Bergaya and Lagaly, 2013). Interlayer cations neutralise the layer
charge of smectite, which is the predominant clay mineral of bentonite
(Gates, 2007; Gates et al., 2009; Likos et al., 2010). Due to its particular
layered structure and charge, montmorillonite can act as a semi-
permeable membrane for charged solutes (ions) (Malusis and
Shackelford, 2002a, 2002b; Shackelford, 2012; Sample-Lord and
Shackelford, 2017; Malusis et al., 2018) and for uncharged solutes
(Grathwohl, 1998), if any are present. The semi-permeable membrane
behaviour of bentonite is, therefore, a combination of solute passage
restriction due to the microstructure and charge of montmorillonite,
and chemico-osmotic flow through pores (Grathwohl, 1998; Malusis
A.S. Acikel, et al.
and Shackelford, 2002a, 2002b; Mitchell and Soga, 2005; Shackelford,
2012; Sample-Lord and Shackelford, 2014, 2017; Tang et al., 2014).
Recent studies on MX80 bentonite and GCLs discussed changes in
cation location and concentration (cmol of cation per kilogram of
bentonite) with increases in (i) salt content (Lu et al., 2018) (ii) water
content and (iii) wetting-drying cycles (Acikel et al., 2019, 2020), and
their impact on changes in matric, osmotic and total suction as well as
bentonite microstructure . First, using a radioactive tracer technique,
Lai and Mortland (1962) investigated the self-diffusion of interlayer
cations in bentonite. They reported that interlayer cations diffused
within inter-layer spaces of oven-dried bentonite and with increasing
water content Na+ migrated from interlayer to inter-aggregate pores
(from micro-to macropores). Later, Acikel et al. (2020) observed cation
self-diffusion phenomenon from interlayer to inter-aggregate spaces on
exhumed GCL specimens after 4 years of exposure to extreme tem-
perature and humidity conditions on site in Antarctica. Acikel et al.
(2020) also reported a total suction increase in exhumed GCL specimens
in comparison to virgin specimens owing to cation self-diffusion.
The pore size of the dialysis membrane prevents PEG from moving
into the soil (bentonite) specimen (Zur, 1966, 1967; Pritchard, 1969);
however, because of semi-permeable membrane behaviour the bento-
nite may also prevent the solute (charged or uncharged) movement into
the PEG solution (Malusis and Shackelford, 2002a, 2002b). Therefore,
at the end of the osmotic tests presented herein, the total suction (not
the matric suction) of the specimen may be equated to the osmotic
suction of the PEG solution. The hypothesis regarding the impact of
membrane behaviour on the suction equilibrium of osmotic suction
control method application is illustrated in Fig. 10. The results reported
in the current study were compared with the total and matric suction
measurements from other techniques reported in the literature. The
results are presented for both wetting (Fig. 11(a)) and drying (Fig. 11
b), paths of GCL3.
Fig. 11(a) shows a comparison of wetting path results from the
current study with wetting path matric suction results from IW-CFPT
(initially wet contact filter paper test) after 4 week suction equilibration
(testing) time (Acikel et al., 2015), matric suction results of high ca-
pacity tensiometer (HCT) tests (Beddoe et al., 2011) and the wetting
path total suction results from chilled-mirror tests (Acikel et al., 2018a).
Similarly, Fig. 11(b) shows a comparison of the drying path from the
current study with those from the drying path matric suction HCT
Fig. 10. A hypothesis of the impact of membrane behaviour of the bentonite component of GCL on osmotic suction control method.
10
Geotextiles and Geomembranes xxx (xxxx) xxx–xxx
reported by Beddoe et al. (2011) as well as those from the drying path
total suction chilled-mirror tests (Acikel et al., 2018a). Acikel et al.
(2018a) investigated different homogenization and testing times to
observe the time dependency of unsaturated GCLs. The result of the
longest water homogenization and testing time tests of Acikel et al.
(2018a) were used for comparison because they represent the highest
degree of the true total suction equilibrium.
Fig. 11 indicates that, while osmotic test results were highly com-
parable with total suction results (by chilled mirror test), they differed
considerably from matric suction results (by IW-CFPT and HCT) for
both wetting and drying paths. These comparative results support the
hypothesis that the osmotic test is a total suction control method ap-
plied to a bentonite-based material such as a GCL owing to the semi-
permeable membrane behaviour of the bentonite to the soluble salts.
4. Conclusions
A modified osmotic suction control technique was successfully used
to obtain GCL wetting and drying path information on an essential
portion of the water retention curves (WRCs). The technique was
modified with a transient monitoring feature, which enabled observa-
tion of the weight change during both wetting and drying paths without
disturbing the test. This modification gave an insight into the actual
wetting and drying paths of the WRCs. The transient gravimetry tech-
nique has a great potential to observe the suction equilibrium paths due
to the bi-modal structure of the bentonite as well as the swelling stages
due to the tri-modal structure of the GCL (the impact of partially con-
fined GCL structure by needle-punched fibres). The monitoring data
supported the proposed conceptual model of time-dependent beha-
viour.
The following are the main conclusions:
1. While the osmotic method is theoretically applicable for suction
control up to 10 MPa, transient monitoring data indicated that the
requirement for the establishment of capillary connections between
the PEG (polyethylene glycol) solution and the GCL specimen means
the technique described herein is not appropriate for GCL samples at
suction values > 2.8 MPa. This value corresponds to the suction
value of 4-layer hydrate state of sodium bentonite (Saiyouri et al.,
2004).
A.S. Acikel, et al.
Fig. 11. Comparison of GCL3 (a) wetting path and (b) drying path water retention test results from different techniques (OT: osmotic test, CM: chilled mirror (Acikel
et al., 2018a), IW-CFPT: initially wet contact filter paper test (Acikel et al., 2015), HCT: high capacity tensiometer (Beddoe et al., 2011)).
2. A hypothesis of the impact of bentonite membrane behaviour on
GCL osmotic testing is presented in this work. The semi-membrane
behaviour of bentonite is postulated to have prevented salts from
moving into the PEG solution during the test. This effect is similar to
how the dialysis membrane prevented the PEG molecules from mi-
grating into the GCL specimen. Hence, when suction equilibrium
was reached between the specimen and the PEG solution, the os-
motic suction due to PEG concentration equalled the total suction of
the GCL specimen instead of matric suction as reported in the tra-
ditional use of the osmotic method. Comparisons of the total suction
results from chilled-mirror technique, matric suction results from
filter paper tests and high capacity tensiometer tests with the results
of the osmotic method support this hypothesis.
3. While tri-modal porosity (macro, meso and micropores) of GCL had
an impact on wetting paths, drying path WRCs were mostly driven
by the bi-modal porosity of the bentonite (macro and micropores)
component.
Current study was a preliminary study on osmotic suction control
monitoring of GCLs, thus the paper focused on qualifying hydration and
dehydration behaviours of GCLs. A future research with an addition of
the volume change monitoring and quantitative comparison with each
total pore volume sizes of tri-modal pore structure will be a very va-
luable.
11
Geotextiles and Geomembranes xxx (xxxx) xxx–xxx
Acknowledgements
This research project was supported by the Australian Research
Council’s Linkage Projects scheme (project number LP0989415). The
authors acknowledge the Australian Government Research Training
Program Scholarship provided to the first author. The support of all the
sponsors is gratefully acknowledged.
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