1042

Hydrogeotechnical characterization of a
metallurgical waste
R. Rodríguez

Abstract: This paper presents the results of hydrogeotechnical characterization tests carried out on the metallurgical
waste (MW) from a tailings impoundment located on the terraces of the Moa River, Cuba. Characterization of the MW
includes chemical and mineralogical analysis, oedometer tests, triaxial tests, tensile strength tests, determination of the
water retention curve, and shrinkage and permeability tests. The MW, which has a grain-size distribution similar to that
of a silt, mainly contains iron and heavy metals minerals and has low plasticity. Consolidated undrained triaxial tests
on remoulded samples indicate a dilative behaviour, with a decrease in pore-water pressure near failure. The material is
susceptible to liquefaction when subjected to a cyclic load in the triaxial test. Hydraulic conductivity, soil stiffness, and
compressive and tensile strength of the MW have an important dependence on the degree of saturation and vary signif-
icantly during the drying process. The results indicate that, during the drying process, cracks in the MW initiate in
quasi-saturated conditions. The cracks increase the hydraulic conductivity by more than one order of magnitude com-
pared with that of intact samples of MW. The main environmental risk with this MW is the possibility of liquefaction
under a cyclic load due to an earthquake and the increase in saturated hydraulic conductivity due to desiccation cracks.
Key words: desiccation cracks, hydrogeotechnical properties, liquefaction, metallurgical waste, characterization.

Résumé : Cet article présente des résultats d’essais de caractérisation hydro-géotechnique effectués sur des déchets mé-
tallurgiques (MW) provenant du réservoir de résidus minier situé sur les terrasses du fleuve Moa, Cuba. La caractérisa-
tion des MW inclut des analyses chimiques et minéralogiques, des essais oedométriques, des essais triaxiaux, des essais
de résistance à la traction, la détermination de la courbe de rétention d’eau ainsi que des essais de retrait et de perméa-
bilité. Les MW présentent un comportement faiblement plastique. La taille des grains correspond à celle d’un silt et ils
contiennent des minéraux ferriques et des métaux lourds. Les essais triaxiaux consolidés non-drainés sur échantillons
remaniés indiquent un comportement dilatant, avec une diminution de la pression interstitielle à l’approche de la rup-
ture. L’échantillon est toutefois susceptible de se liquéfier sous charge triaxiale cyclique. La conductivité hydraulique,
la rigidité du sol, la résistance à la traction et à la compression des MW dépendent fortement du degré de saturation et
peut varier de façon significative pendant le séchage. Les résultats indiquent que les fissures dans les MW commencent
en conditions quasi-saturées. Les fissures augmentent la conductivité hydraulique de plus d’un ordre de grandeur par
rapport à celle des échantillons intacts de MW. Le risque écologique causé par les MW est donc relié à la possibilité
de liquéfaction en présence d’une charge cyclique causée par un séisme et à l’apparition de fissures de dessiccation qui
augmentent leur conductivité hydraulique.
Mots clés : fissures de dessication, propriétés hydro-géotechniques, liquéfaction, résidus métallurgiques, caracterisation.

Rodríguez 1060

Introduction ings from Fe (oxy)hydroxy minerals from lateritic deposits

The majority of the studies of mine and metallurgical
wastes (MW) have focused on the geochemical and mineral-
ogical behaviour of the wastes (Swarbrick and Fell 1992;
Ribet et al. 1995; Vick 1996). According to a literature re-
view, the available information on the geotechnical proper-
ties of MW is usually on wastes from hard-rock mines (e.g.,
Markland and Eurenius 1976; Aubertin et al. 1994, 1996;
Barrera and Lara 1998; Dawson et al. 1998; Chapuis and
Aubertin 2003). Limited data have been found on MW tail-
Received 24 March 2003. Accepted 26 April 2006. Published
on the NRC Research Press Web site at http://cgj.nrc.ca on
1 November 2006.
R. Rodríguez. Department of Geotechnical Engineering and
Geosciences, Technical University of Catalonia (UPC),
Barcelona, Spain (e-mail: roberto.rodriguez@udg.es).
Can. Geotech. J. 43: 1042–1060 (2006) doi:10.1139/T06-061
(Heredia 1980; Rodríguez et al. 1998a, 1998b; Tibana and
De Campos 1998; Rodríguez 2002a, 2002b). The environ-
mental impact on surface water and groundwater has been
analysed by different authors (Szymanski and Macphie
1994; Younger 1999; Rodríguez et al. 2000; Rodríguez and
Candela 2004).
As a result of the metallurgical process, water-borne slur-
ries are generated and deposited in a liquid form into a spe-
cific area bounded by tailings impoundments. These
materials are initially saturated but desiccate when exposed
to certain climatic conditions (temperature and wind). Desic-
cation induces volume and stress changes in the MW, lead-
ing to vertical fissures. Depending on the geological material
and subsequent metallurgical process, MW is typically char-
acterized by a grain-size distribution between 0.01 and
1 mm and a particle density between 1.50 and 4.00 g/cm3
(Blight 1994; Vick 1996; Gipson 1998; Rodríguez et al.
© 2006 NRC Canada
Rodríguez
1998a). The mineralogy and chemical composition of MW
are highly variable, depending on the orebody type and met-
allurgical process, but (Fe, Al) (oxy)hydroxide minerals, sul-
phide minerals, quartz, and clay minerals are the most
prevalent. According to several authors (Markland and
Eurenius 1976; Ribet et al. 1995; Vick 1996; Tibana and De
Campos 1998; Rodríguez et al. 1998a, 1998b), the internal
friction angle may range between 27° and 41°, and the void
ratio, e, between 0.8 and 3.6.
In general, MW slimes show low strength, low permeabil-
ity, and low compressibility, and low consolidation rates
have been also reported (Vick 1996). They exhibit little or
no effective cohesion and can be susceptible to liquefaction
under seismic loading during earthquakes or cyclic triaxial
tests (Troncoso 1988; Yasuhara et al. 1994; Vick 1996;
Barrera and Lara 1998; Rodríguez 2002a).
Theoretical and experimental analyses of desiccation
cracks in cohesive and plastic soils have been carried out by
several researchers (e.g., Blight 1971, 1997; Miller 1975;
Snyder and Miller 1985; Towner 1987a, 1987b; Morris et al.
1992; Swarbrick and Fell 1992; Abu-Hejleh and Znidarcic
1995; Drumm et al. 1997; Konrad and Ayad 1997; Kodikara
et al. 2000; Yesiller et al. 2000); however, limited informa-
tion has been found on this phenomenon in low-
plasticity MW (Heredia 1980; Lloret et al. 1998).
The aim of the paper is to present the physical, mechani-
cal, and hydrogeotechnical characteristics of a specific MW
and the influence of desiccation cracks on its hydraulic con-
ductivity. This study constitutes a necessary step in the anal-
ysis of the influence of desiccation cracks on preferential
flow and heavy-metal transport to underlying aquifers and
the analysis of the stability of the tailings impoundment.
Site description
The Moa mining district in northeastern Cuba (Fig. 1) has
become one of the most important centres in the world for
the production of nickel and cobalt (oxidized–hydroxidized
species) from lateritic orebodies (Anthony and Flett 1997).
The area is characterized by temperatures between 24 and
27 °C and high rainfall (average 1800 mm/year, exceeding
2000 mm in some years). There is some seismic activity in
the area, with estimated recurrence periods of 60–80 years
for earthquakes of magnitudes greater than 7 (Rodríguez et
al. 1996; Cotilla 1998).
Mineral exploitation began near Nicaro in 1943, and
20 years later in the Moa area (Fig. 1). Tailings are accumu-
lated in a specific area bounded by five impoundments and
cover an area of about 10 km2, with the thickness of the de-
posit ranging between 6 and 20 m at Nicaro and between 4
and 8 m at Moa. The solid material deposited accounts for
more than 180 million tonnes.
The Moa mining district is the only region in the world
where acid leaching (SAL) and Caron-type (ACL) industrial
processes for the extraction of Ni and Co from lateritic de-
posits coexist. The Caron-type process refers to ammoniacal
ammonium carbonate leaching (ACL) with oil addition, and
SAL refers to sulphuric acid leaching (Ponjuan and
Rodríguez 1981; Anthony and Flett 1997). The MW produc-
tion rate from the two processes is 5200 t/day (UNI 1994),
which is hydraulically transported by pipelines and depos-
1043
ited in the storage area. The slurry of MW transported by
pipelines is 30%–40% solid and 70%–60% liquid (see
Fig. 2c).
The mining activity and the MW have had several impor-
tant environmental impacts in the area, among them heavy-
metal pollution of surface water (Rodríguez et al. 1998a,
1998b; Rodríguez 2002b), groundwater pollution with heavy
metals and sulphate (Rodríguez and Candela 1998), pollu-
tion of sea water (González and Ramírez 1995), and pollu-
tion of a coral barrier (Martínez et al. 1993).
Material
In April 1996, ten 2 kg samples of MW were collected
and analysed for their physicochemical and mineralogical
properties in tailings impoundments 3 and 5 (five samples
per impoundment, Fig. 1). The 10 samples for chemical
analysis were sealed in plastic bags and kept under refrigera-
tion (temperature 6–8 °C) until they were tested in the labo-
ratory. Five more MW samples (-20 kg) were collected at
different locations on the tailings surface of the Moa im-
poundment (tailings impoundment 3, Fig. 1) and used for
mechanical and hydrological analysis. These samples were
sealed in plastic bags, but not kept under refrigeration so
that their physical properties were not changed.
Method
Physical, mineralogical, and chemical characterization
Grain-size distribution of samples was obtained by means
of a laser technique using Malvern Mastersize/E equipment
(range 0.5–600 µm) (Rodríguez 2002a). The X-ray diffrac-
tion technique was used to characterize the minerals present
in the tailings. X-ray diffraction tests were conducted in a
Siemens D-5000 diffractometer with a Bragg-Brentano θ:2θ
configuration, using a Cu target tube and a graphite mono-
chromator, operating at 40 kV and 20 mA. Samples were
analysed within the 4°–60° range, taking data every 0.05°
with a step-time of 3 s. X-ray diffraction plots were studied
using the Siemens automatic software for peak recognition,
mineral identification, and peak intensity calculations.
The chemical composition of the samples was determined
by digestion of 2 g of MW with acid at different acid to soil ra-
tios (1:3 HNO3; 1:5 HClO4; 1:3 HF). Nineteen elements (Fe,
Cr, Ni, Mn, Zn, Cu, Ni, Co, Al, Mg, Ca, Ba, Sr, Pb, Cd, Ag,
Hg, P, Au) were analysed from the final solution by inductively
coupled argon plasma – atomic emission spectrometry (ICP–
AES) and inductively coupled plasma – mass spectrometry
(ICP–MS). Oxidizable organic matter (OM) was calculated by
the electrochemical volumetric method (Buurman et al. 1996).
The Gilman method for acid soil was applied to determine
the cation exchange capacity (CEC). For the pH measure-
ment, deionized water was added to a waste sample at a
waste to water ratio of 1:2.5 (Page 1986).
Mechanical characterization
A series of mechanical tests on remoulded samples was
carried out, including oedometer tests, unconfined compres-
sion tests, extension tests, and triaxial tests (ASTM 1993).
Cyclic triaxial tests were also performed to assess the lique-
faction potential of the MW. The mechanical characterization
© 2006 NRC Canada
1044
Fig. 1. Location of the Moa and Nicaro mining districts, Cuba, and the existing tailings impoundments. Impoundments 1, 2, and 3 cor-
respond to an ammonium carbonate leaching process (ACL) with oil addition, and impoundments 4 and 5 to a sulphuric acid leaching
(SAL) process.
was performed under saturated and unsaturated conditions to
determine the physical parameters that control water flow
through the MW and the development of desiccation cracks.
The properties of different samples of MW used in the me-
chanical tests are listed in Table 1.
Undrained and cyclic triaxial tests were performed in a
Triaxial GDS (Imperial College type stress path cell), with
automatic data acquisition (GDS Instruments Ltd., Hook,
UK). The instrumentation used comprised an internal load
cell and pore pressure, cell pressure, external axial displace-
ment (±100 mm), and volume change transducers. Pore pres-
sures were measured with transducers attached to the base
and top of the triaxial cell.
The tensile strength for different degrees of saturation was
measured for three different densities (1.32, 1.44, and
1.53 g/cm3) using a device similar to those described by
Mikulitsch and Gudehus (1995), Lloret et al. (1998),
Rodríguez (2002b), and Kim and Hwang (2003).
Hydrogeotechnical characterization
Hydrogeotechnical characterization is very important for
future analyses of pollution transport in the deposition areas
themselves. This work focuses on the hydrogeotechnical
characterization of ACL MW in the Moa mining district,
Cuba. Because of the lack of previous characterizations
of MW, standard hydrogeotechnical tests (liquid and plastic
limit, saturated and unsaturated hydraulic conductivity, satu-
rated oedometer and collapse in homogeneous samples) and
modified hydrogeotechnical tests (e.g., saturated hydraulic
conductivity in layered and cracked samples with different
thicknesses) were performed (ASTM 1993). Additional tests
Can. Geotech. J. Vol. 43, 2006
related to the material parameters under unsaturated condi-
tions were also carried out. A series of MW water retention
curves were obtained using different procedures (transistor
psychrometer, oedometer test with suction control, salt solu-
tion) according to the suction range considered. These
curves are described later in the paper.
A transistor psychrometer (Dimos 1991) was used for to-
tal suctions between 0.1 and 10.0 MPa. In this case, samples
(30 small cylinders, 15 mm in diameter, 12 mm in height,
and with three different densities of 1.32, 1.44, and
1.53 g/cm3) were compacted with an initial water content to
achieve a given dry density. When analysing wetting pro-
cesses, saturated samples were initially dried by applying a
suction of 38 MPa using an NaCl salt solution for 90 days.
Water was added drop by drop to each sample (Rodríguez
2002b; Lloret et al. 2003). The suction was measured with a
12-channel transistor psychrometer (Dimos 1991; Rodríguez
2002a; Lloret et al. 2003).
The behaviour of samples for suctions lower than 1 MPa
was studied using an oedometer test with suction control
(Rodríguez 2002b; Lloret et al. 2003). The apparatus al-
lowed evaluation of the changes in volume and water con-
tent of the sample with changes in suction or vertical load
under unsaturated conditions. The oedometer (Lloret and
Alonso 1985) uses the axis-translation technique (Hilf 1956)
to control the matrix suction of the MW. Vertical stress was
kept constant at 0.03 MPa during the tests. Suction varia-
tions were imposed applying an air pressure of 1 MPa to the
upper end of the sample (50 mm in diameter, 20 mm in
height, and dry densities of 1.32, 1.44, and 1.53 g/cm3) and
varying the water pressure on the high air entry value (AEV)
© 2006 NRC Canada
Rodríguez 1045

Fig. 2. (a) Desiccation cracks at impoundment 5. (b) Desiccation cracks at impoundment 3. (c) Metallurgical wastes (MW) discharge
and beach deposition in tailing dam, observe the estratification in MW with different thicknesses. Area in each photograph is approxi-
mately 1 m2, with notebook and pen for scale.

porous stone at the base. Measurement of the amount of wa-
ter entering or escaping the sample allows the water content
to be controlled. Performing this measurement over time, the
unsaturated permeability can be estimated from the water
content evolution for a given change in suction. This re-
quires back-analysis with the simplified Richards model,
taking into account the low permeability of the porous stone
with its high AEV (Kunze and Kirham 1962).
Desiccation cracks: sample preparation
The in situ desiccation process in tailings ponds induces
volume and stress changes in the MW, which generates ver-
tical fissures 20–80 cm deep and more than 5 cm wide
(Figs. 2a, 2b). Due to different deposition events and differ-
ent dry cycles it is possible to observe the stratification and
desiccation cracks in the deposit (Fig. 2c). To observe crack
generation due to desiccation processes, five drying tests
were performed with MW covering a circular plate (225 mm
in diameter). This type of test is similar to that described by
Lloret et al. (1998) and Kodikara et al. (2000). The plates
were grooved to a depth of 1.5 mm to avoid slippage be-
tween the plate and the MW (Fig. 3a). The MW was depos-
ited on the plates in different thicknesses (4, 8, and 16 mm)
and with an initial gravimetric water content of 50%, an ini-
tial porosity of 0.66, and a dry density of 1.33 g/cm3. Four
series of tests were performed in hermetic containers (with

© 2006 NRC Canada

1046 Can. Geotech. J. Vol. 43, 2006

Table 1. Principal characteristic of the sample of MW for different hydrogeotechnical tests made in this study.
Diameter Height Dry density
Tests (mm) (mm) (g/cm3)
Conventional oedometer tests 50 20 1.39
Collapse oedometer tests 50 20 1.39
Unconfined compression tests 38 76 1.53
Tensile stress tests 38 20 1.53
Triaxial tests 38 76 1.53
Cyclic triaxial tests 38 76 1.53
Suction measurement (psychrometric method) 15 12 1.58
15 12 1.44
15 12 1.32
Oedometer with suction control 50 10 1.53
Shrinkage limit tests 38 76 1.53
Hydraulic conductivity tests, homogeneous samples 100 120 1.53
Cracks samples with three types of layers, 10, 20, and 40 mm thick 100 120 1.53

Fig. 3. (a) System used for desiccation tests with different boundary conditions. 1, suction control solution; 2, scale; 3, sample of
waste placed on circular plate; 4, displacement transducer; 5, hygrometer. (b) Method used to measure distance between cracks, area,
and perimeter of waste samples. All measurements in millimetres.

capacities of about 12 L, Fig. 3a) where the relative humid-
ity of the air was imposed using saline solutions with so-
dium chloride or sulphuric acid (Rodríguez 2002b; Lloret et
al. 2003). In a fifth series, the plates remained open to the
laboratory atmosphere with a 60% relative humidity. The psy-
chrometric law (Fredlund and Rahardjo 1993) relates the final
suction of the water in MW to the relative humidity of the at-
mosphere surrounding the sample, “assuming equilibrium”.
Temperature was held constant at 22 ± 2 °C, and relative hu-
midity and temperature were measured with a hygrometer
(Fig. 3a). The shrinkage of the MW was measured with a dis-
placement transducer (Fig. 3a). When the desiccation tests
were complete, a picture was taken and analysed with
AutoCAD® (Autodesk Inc., San Rafael, Calif.). The perime-
ter of the crack and the distance between two crack planes
were measured (Fig. 3b). The average distance between the
different crack planes was determined for all samples.
Effect of desiccation cracks on hydraulic conductivity:
sample preparation
To analyse the effect of desiccation cracks and stratifica-
tion on the flow and transport of contaminant, four col-
umns were made in the laboratory. After mixing the waste
material with distilled water (56% water and 44% solid ma-
terial) to simulate the sedimentation process at the mining
site, it was placed in this slurry state in a large column
(300 mm in diameter and 120 mm high). Four columns
with similar physical characteristic were tested. The first
three columns were constructed step-by-step in a stratified
way. The volume of material deposited in each column

© 2006 NRC Canada

Rodríguez 1047

Table 2. Mineralogical composition of the wastes in percentage of total weight.

Tailings impoundment Tailings impoundment Tailings impoundment
Mineral 1 (n = 10) 3 (n = 5) 5 (n = 5)
Magnetite, (Fe)Fe2O4 0.5–1.3 3.0–8.0 0.6–1.2
Hematite, Fe2O3 62–70 60–70 69–75
Quartz, SiO2 1.5–3.9 2.0–4.2 1.3–3.1
Gibbsite, Al(OH)3 1.8–5.2 1.0–3.0 1.4–6.0
Anatase, TiO2 0.05–0.06 0.03–0.06 0.04–0.05
Alunite, H3OAl(SO4)2(OH)6 9.0–13.4 8.9–14.0
Gypsum, CaSO4·H2O 0.01–0.10 0.10–1.20 2.50–5.60
Serpentine, Mg3Si2O5(OH)4 0.3–1.2 0.6–1.4
Chrome spinel, MgCr2O4 3.1–3.8 2.0–4.0 2.1–2.8
Magnesioferrite, (Mg)Fe2O4 0.1–3.0
Note: n, number of samples.

Table 3. Concentration of selected elements in the waste.

Elements (% of total weight; n = 5)
Eh CEC OM (% of
pH (mv) (mequiv./100 g) total weight) Ti Mn Al Fe Co Zn V Ni Ba Cr
SAL 4.1 422 8.5 4.5 0.57 0.42 4.94 43.58 0.03 0.01 0.03 0.18 0.0028 0.53
ACL 6.5 325 8.0 0.6 0.06 0.72 4.80 49.19 0.10 0.05 0.03 0.60 0.0030 1.72
Note: n, number of samples; OM, organic mater.

Fig. 4. Grain-size distribution of ACL MW obtained by a laser
technique.
gave more or less homogeneous layers with different thick-
nesses (approximately 10, 20, and 40 mm). Only when the
previous layer had cracked and consolidated was the fol-
lowing layer placed. The drying process was produced by
applying similar climatic parameters from the study area to
the column surface for 1 week (in each layer). For this
case, the climatic boundary conditions were a temperature
of 26 ± 0.5 °C and a relative humidity of 60 ± 5%. During
the drying process in a stratified column, cracks were pro-
duced on the top of the deposited layers. In each test, vol-
ume and porosity variations due to shrinkage were con-
trolled. The shrinkage and change in thickness were mea-
sured using a displacement transducer similar to that shown
in Fig. 3a. A photograph was taken when the desiccation
test was finished, the area and volume of cracks were mea-
sured, and the distribution of cracks was drawn using
AutoCAD® (Fig. 3b).
In the second test, the MW material prepared with the
same initial water content was placed all at once, forming a
column with the same height, and was then desiccated fol-
lowing the same procedure as that for the layered column.
When the previous four columns were desiccated and their
total heights were calculated, one sample (100 mm in diame-
ter, 120 mm high) in each column was taken to measure the
hydraulic conductivity.
The initial average dry density for stratified columns
with 10, 20, and 40 mm thick layers was different in each
sample (1.38, 1.32, and 1.24 g/cm3, respectively; and
1.40 g/cm3 in homogeneous samples). Each sample was put
in a triaxial cell. To avoid preferential flow through the
walls, the columns were covered with a rubber membrane.
In the triaxial cell the sample was saturated for 48 h, with a
confining pressure of 5 kPa and a hydraulic gradient of 0.1.
When the sample was totally saturated, the samples were
consolidated to achieve a density of 1.53 g/cm3. The
change in porosity of the sample in the saturated condition
was controlled by measuring the amount of water that en-
tered (wen) and escaped (wes) from the sample. The differ-
ence between wen and wes represents the change in volume
of the sample. The dry density and porosity were calculated
using this change in volume. When the difference between
volumes of water entering and escaping became zero, the
hydraulic conductivity was measured for 24 h in each sam-
ple of MW.

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1048 Can. Geotech. J. Vol. 43, 2006

Table 4. Basic characteristics of the mine tailings materials (n = number of samples).

Tailings impoundment Tailings impoundment Tailings impoundment
Parameter 1 (n = 22)a 3 (n = 6) 5 (n = 20)a
Natural density (g/cm3) 2.15–1.73 2.38–2.29 2.38–2.23
Dry density (g/cm3) 1.57–1.33 1.83–1.64 1.83–1.67
Particle density (g/cm3) 4.11–3.52 3.80–4.04 3.99–3.77
Water content (%) 30.9–25.0 35.00–25.00 35.30–29.40
Liquid limit 40.4–35.3 44.0–40.0 25.0–23.0
Plastic limit 36.8–30.0 40.0–36.0 24.0–21.0
Plasticity index 7.4–3.1 6.0–4.0 11.0–6.0
Void ratio 1.95–1.47 2.20–1.30 1.35–1.15
a
Data from Heredia (1980).

Fig. 5. Conventional saturated oedometer and collapse tests on
statically compacted waste. Collapse obtained when wetting un-
saturated samples under constant loads. Vertical bars represent
the consolidation of dry material when is saturated.
sity of about 2.30 g/cm3, a particle density between 3.80 and
4.04, and a void ratio between 1.3 and 2.2. The liquid limit
is between 40 and 44, and the plastic limit about 36–40.
The MW shows a low plasticity index between 4 and 6. The
absence of clay minerals gives the MW low plasticity. Ac-
cording to the grain-size distribution, MW can be catego-
rized as a sandy silt (class ML following the Unified Soil
Classification System). Table 4 summarizes some of the
most relevant physical parameters of the MW from the in-
vestigated tailings impoundment 3 and presents physical
characteristics obtained in situ by Heredia (1980) from MW
in tailings impoundments 1 and 5 (Fig. 1). In situ density for
the three tailings impoundments oscillates between 1.78 and
2.38 g/cm3, with an average value of 2.19 g/cm3, and gravi-
metric water content is between 25.0% and 35.0%, with an
average value of 32.8%. The void ratio varies between 1.1
and 2.2 (Table 4). The MW reaches full saturation during
rainy periods, whereas in dry periods, below a superficial
crust, the degree of saturation varies according to the
weather (Fig. 2).

Mechanical characteristics

Results and discussion
Mineralogical, chemical, and physical characteristics
The mineralogical study indicates that the main compo-
nents of the waste are iron and (oxy)hydroxide minerals, es-
pecially hematite (60%–75%) and magnetite (1%–8%).
Secondary minerals are quartz (1%–3%), gibbsite (1%–6%),
and magnesioferrite (0.1%–3.0%). The results of the mineral-
ogical analyses are summarized in Table 2. The chemical
composition is given in Table 3. In general, the waste is
mainly composed of iron and heavy metals: Fe (40–50 wt.%),
Cr (1–3 wt.%), and Mn (1–2 wt.%).
The ACL MW presents an almost neutral pH (6.5), and
the SAL MW presents an acidic pH (4.1). A CEC was ob-
tained of 8 mequiv./100 g of solid waste, which is consistent
with values reported in the literature for (oxy)hydroxides of
Fe, Al, and Cr (Sparks 1995).
According to the grain-size distribution shown in Fig. 4,
99% of the residue has a grain size finer than 0.2 mm, with a
mean grain size of 20 µm. The material has an in situ den-
Oedometer tests
Figure 5 shows the results of the oedometer tests on
remoulded samples of ACL MW at an initial water content
of 44% (tailings impoundment 3, Fig. 1) statically com-
pacted to a dry density of 1.39 g/cm3. Under these condi-
tions, the samples are saturated, the compression index (Cc)
obtained is 0.26, and the swelling index (Cs) is 0.05. The
stiffness of these remoulded samples is lower than that mea-
sured by Heredia (1980) for undisturbed samples. Some
compacted samples were air dried in the laboratory atmo-
sphere, reaching an average water content of only 3%. When
a sample with that initial water content is loaded, its com-
pressibility is lower than that under saturated conditions
(Cc = 0.12). Nevertheless, when samples with that initial wa-
ter content are saturated under a constant load, an important
reduction in volume (collapse) takes place and the samples
reach a final void ratio similar to that corresponding to
loaded samples that were initially saturated. In Fig. 4 the
magnitude of the collapse strains for different vertical con-
stant loads can be observed. This behaviour is consistent
with that observed in natural soils with a grain-size distribu-
tion and porosity similar to those of the MW (Alonso et al.
1987).

© 2006 NRC Canada

Rodríguez
Fig. 6. (a) Young’s modulus (E) for different degrees of saturation. (b) Uniaxial compressive strength (curve I) and tensile strength
(curve II) for different degrees of saturation.
Unconfined compression tests
Unconfined compression tests were performed on samples
statically compacted to three dry densities (1.32, 1.44, and
1.53 g/cm3). Under these conditions, the samples were ini-
tially saturated. The samples were dried in a laboratory-
controlled atmosphere (relative humidity of 60 ± 5% and
temperature of 22 ± 2 °C), reached different final water con-
tents, and became unsaturated. Figures 6a and 6b (curve I),
respectively, show the influence of the degree of saturation
on the value of Young’s modulus and the unconfined com-
pression strength measured in the tests. A clear increase in
stiffness can be observed when the material becomes drier.
Apparently, the maximum value of unconfined compression
strength corresponds to a degree of saturation between 80%
and 90% in the water retention curve (see Fig. 9).
Tensile strength
The tensile strength of the samples prepared under the
same initial moisture conditions as those for the samples
used in unconfined compression is measured using a device
similar to that described by Mikulitsch and Gudehus (1995).
The measured tensile strength is plotted in Fig. 6b (curve II).
The unconfined compression and tensile strength gave maxi-
mum values for a degree of saturation of about 0.8–0.9. The
ratio of the maximum compressive strength to the maximum
tensile strength is about five and is generally the same for
three different dry densities (1.32, 1.44, and 1.53 g/cm3) be-
cause the material has no cohesion and the internal tensile
strength depends on the optimal water content. The result
obtained for the saturation condition (Sr = 1) is in agreement
with the results of Nearing et al. (1991), who studied 33 sat-
urated repacked soils and obtained tensile strength values
between 1.00 and 3.23 kPa, which are similar to those ob-
tained for MW (see Fig. 6b).
The results of the tests of tensile strength and uniaxial
compressive strength obtained from MW samples present a
similar trend for three different densities. They reach maxi-
1049
mum values for degree of saturation between 0.8 and 0.9
(Fig. 6b). The tensile strength of fine-grained soils depends
on the interparticle attraction, which depends on the cohe-
sion of the material and the water content. In this case, how-
ever, the material has no cohesion. Once the degree of
saturation reaches 90%, the tensile strength and unconfined
compression decrease very rapidly (Fig. 6b).
Undrained triaxial tests
Undrained triaxial compression tests (isotropically consol-
idated) were performed on the same type of specimens as
those used in the compression tests. The tests were carried
out on saturated samples for different vertical stress, σ1′ (650,
700, 800, and 950 kPa), and initial effective confining
stresses, σ3′ (50, 100, 200, and 350 kPa). The results given in
Fig. 7 are obtained for Sr = 1 and show that there are large
increments of pore-water pressure for small axial deforma-
tions (smaller than 2%), whereas the material shows dilative
behaviour and pore pressures reduce when the strains are
larger than 2% (Fig. 7b). The angle of internal friction de-
rived from these tests is 35.6° (Fig. 7c). This behaviour is
similar to that observed by Tibana and De Campos (1998)
for loose iron tailings.
Cyclic triaxial tests
Stress-controlled cyclic triaxial tests were performed un-
der undrained conditions on saturated samples with an initial
dry density of 1.53 g/cm3. Figure 8a presents the relation-
ship between the number of cycles necessary to achieve liq-
uefaction and the value of the cyclic stress ratio, σd /(2σ3′ ),
where σd is the cyclic stress amplitude, and σ3′ is the initial
effective confining stress. Figure 8a also presents the num-
ber of cycles necessary to reach different values of axial
strain for a given stress ratio and shows that, once liquefac-
tion is reached, the deformations tend to grow rapidly. Fig-
ure 8b shows that pore pressures (u) start to increase when
the axial strain reaches values of about 0.1% and becomes
© 2006 NRC Canada
1050
Fig. 7. (a) Stress paths of conventional triaxial compression tests. (b) Relationship between pore-water pressure and axial deformation
for different confining effective stresses. (c) Plot of the mean effective stress (p′) versus deviator stress (q) relationship for large
strains. φ, angle of internal friction.
equal to the effective confining stress for axial strains of
about 1% for all cases (irrespective of the confining stress).
These results are consistent with those from Dobry presented
by the National Research Council Committee on Earthquake
Engineering (1985) from strain-controlled triaxial tests on
sands of diverse origins and relative densities.
Hydrogeotechnical characterization
Water retention curves
Hydrogeotechnical characterization is very important for fu-
ture analyses of pollution transport in the actual deposition ar-
eas. Figure 9a shows the water retention curves (WRC)
corresponding to the drying and wetting processes for samples
with an initial void ratio (eo) of 1.75. The results show a very
important hysteresis in the retention curve, and the wetting pro-
Can. Geotech. J. Vol. 43, 2006
cess shows a significant reduction in suction for an identical
degree of saturation. Measurements performed with psychro-
meters are consistent with those obtained in the oedometer test,
which indicates that the total suction measured with psychro-
meters is similar to the matric suction imposed with the oedo-
meter. The retention curve shows that the residual degree of
saturation is approximately between 8% and 12%.
Figure 9b shows the effect of the initial void ratio (eo) on
the retention curve for drying tests. A reduction in the initial
void ratio implies a significant increase in the AEV of the
material. In the WRC, the AEV is defined as the matric suc-
tion at which air first enters the largest pores of the soil dur-
ing a drying process (Brooks and Corey 1964, 1966).
Table 5 shows the estimated AEV for different dry tests
according to the tangent method (Fredlund and Xing 1994;
Aubertin et al. 2003; Yang et al. 2004). The AEV in MW is
© 2006 NRC Canada
Rodríguez
Fig. 8. (a) Cyclic stress ratio versus number of cycles to reach liquefaction for a given axial strain. (b) Ratio of pore-water pressure, u,
and initial confining stress, σ3′, versus vertical strain.
Fig. 9. (a) Water retention curves for drying and wetting paths
(free volume conditions) for an initial void ratio of 1.75. (b) Water
retention curve for drying paths and different initial void ratios.
similar to that obtained by Aubertin et al. (1998) using tail-
ings from hard-rock mines.
Figure 10 shows the change in volume and water content
experienced by the MW in different suction steps. The vol-
ume increases during the suction-controlled oedometer test.
In the first case (Figs. 10a, 10c), with an increase in suction
of between 0.01 and 0.03 MPa, the sample, due to the low
1051
Table 5. Degree of saturation and air entry value for water reten-
tion curves at different initial void ratios.
Initial void ratio, eo
1.50 1.75 2.00
Path Drying Drying Drying
Air entry value, AEV (MPa) 0.389 0.144 0.041
Degree of saturation, Sr 0.99 0.99 0.99
value of the applied suction, remains practically saturated
and the change in total volume is very similar to the water
loss. When the suction increment is higher (from 0.4 to
0.6 MPa, Figs. 10b and 10c), however, the sample has a
smaller degree of saturation, and the change in total volume
of the sample is very small compared with the change of wa-
ter volume, indicating that air replaces the water lost from
the pores.
Shrinkage and desiccation cracks of metallurgical waste
(MW)
Shrinkage limited
Figure 11 presents the evolution of the void ratio and the
degree of saturation of the sample during a cycle of drying–
wetting–drying performed under a constant vertical load of
0.03 MPa in the suction-controlled oedometer. An important
irreversible deformation can be observed during the first cy-
cle of drying, whereas in the subsequent cycles the strains
are smaller and practically reversible. It should be pointed
out that most of the volumetric strains take place while the
material is saturated (suctions smaller than 0.1 MPa), but
volume changes are already very small for suctions higher
than 0.2 MPa. The shrinkage limit can be estimated from
Fig. 11b to be in the gravimetric water content range of
37%–39%.
Figure 12 shows the evolution of the volumetric strain
with volumetric water content for an initially saturated cylin-
drical specimen (38 mm in diameter and 76 mm in height).
The initial dry density was 1.33 g/cm3, and the sample was
exposed without confinement to an atmosphere with a rela-
© 2006 NRC Canada
1052
Fig. 10. Sample volume change and water exchange for first drying path: (a) suction increments from 0.01 to 0.03 MPa; (b) suction
increments from 0.40 to 0.60 MPa; (c) change in solid and water volume for different suctions and times.
tive humidity of 60% and a temperature of 22 ± 2 °C. It is
observed that the relationship between the change of volume
(measured as the change in the dimensions of the specimen)
and the volumetric water content (obtained from weighing)
is linear for high water contents. The shrinkage limit, wr, re-
sulting from the final deformation is about 0.37. It should be
pointed out that in the oedometer tests and in this shrinkage
test, the change in volume experienced by the MW in satu-
rated conditions is large (Figs. 10–12).
Desiccation cracks
A series of drying tests with MW placed on circular plates
(225 mm in diameter) was performed to observe crack gen-
eration due to desiccation processes. Table 6 summarizes the
main characteristics of all the tests. Figure 13 shows three
photographs corresponding to tests carried out with three
different thicknesses of MW (4, 8, and 16 mm), with each
sample placed in hermetic containers imposing a relative hu-
Can. Geotech. J. Vol. 43, 2006
midity of 75%. It should be pointed out that the thicker the
sample, the longer the distance between fissures.
Some results corresponding to these tests and referring to
crack formation are presented in Fig. 14 and Table 6. Fig-
ure 14a presents the measured relationship between sample
thickness and distance between cracks. The average distance
between cracks is determined by measuring the separation
between two continuous planes of desiccation cracks. The
process was carried out for all samples, and the average
value was calculated (Fig. 3b). The width of the cracks is
variable (0.05–1.30 mm) and depends on sample thickness
(Table 6). It should be noted that this relationship is almost
linear, and the imposed suction only plays a secondary role.
Figure 14b shows the gravimetric water content measured
when cracks initiate. It can be seen that this water content is
quite high for imposed suctions smaller than 60 MPa, which
implies that samples are unsaturated. For higher suctions,
however, the measured water content at the initiation of
© 2006 NRC Canada
Rodríguez
Fig. 11. Evolution of the void ratio and degree of saturation of the sample during a cycle of drying–wetting–drying performed under a
load of 0.03 MPa in the suction-controlled oedometer: (a) void ratio change versus prescribed suction; (b) shrinkage curve; (c) water
retention; (d) degree of saturation versus water content.
Fig. 12. Volumetric strain versus water content (compacted sam-
ple with diameter 38 mm, height 76 mm, and dry density
1.53 g/cm3). Shrinkage limit (wr) is around 0.37. ∆V, change of
the volume; Vo, initial volume.
1053
cracks is smaller than the shrinkage limit. This behaviour
can be explained by an increase in the tensile strength with
an increase in suction.
Figure 14c shows the time required for cracks to initiate
for a given suction. In general, the higher the suction, the
shorter the time required. The time to crack initiation also
increases with an increase in sample thickness. Solid sym-
bols in Fig. 14 refer to samples open to the laboratory atmo-
sphere that do not follow this general pattern. This could be
due to the larger air volume available for exchange com-
pared with the volume available in the hermetic containers.
The gravimetric water content in samples when cracks begin
is very high and suction is very low. According to the
gravimetric water content in all samples, the saturation de-
gree is between 0.80 and 0.96; for this value, the suction
in MW is lower than 0.1 MPa considering the retention
curve (Fig. 9). These results show that the samples were not
in equilibrium with the salt solution when cracks appeared.
Desiccation cracks appeared for a degree of saturation be-
tween 0.80 and 0.96 (see Fig. 9). Vertical strain measured
with the displacement transducer is more pronounced under
laboratory atmospheric conditions than in the hermetic con-
tainers and increases when the prescribed suction and sam-
ple thickness also increase (Fig. 14d).
Figure 15 shows the loss of water versus time for different
tests under laboratory atmosphere conditions (open system)
© 2006 NRC Canada
1054 Can. Geotech. J. Vol. 43, 2006

Table 6. Sample characteristics of desiccation tests in a controlled atmosphere for open and closed systems.

Time to Gravimetric Final Distance Vertical

Imposed Imposed Initial dry Soil crack water content crack between strain at Final
relative suction density thickness initiation at crack opening cracks crack vertical
humidity (%) (MPa) (g/cm3) (mm) (days) initiation (%) (mm) (mm) initiation (%) strain (%)
Hermetic container
97.8 3.0 1.33 4 22.00 41.9 0.40 17 1.1 1.2
3.0 1.33 8 35.00 43.5 0.80 37 1.4 1.5
3.0 1.33 16 58.00 43.7 1.20 117 1.5 1.7
75.0 38.0 1.33 4 9.00 42.6 0.10–0.50 14 2.7 3.0
38.0 1.33 8 15.00 43.8 0.10–0.60 39 3.0 3.1
38.0 1.33 16 26.00 45.9 0.10–0.80 55 2.4 2.5
60.0 58.9 1.33 4 6.00 41.9 0.10–0.50 14 4.9 5.2
58.9 1.33 8 12.60 43.5 0.05–0.60 30 6.1 6.4
58.9 1.33 16 19.50 43.1 0.05–1.30 66 5.6 5.7
15.6 251.0 1.33 4 3.00 29.6 0.05–0.10 14 7.8 8.0
251.0 1.33 8 10.00 30.1 0.05–0.50 36 7.2 7.5
251.0 1.33 16 14.00 30.5 0.05–1.20 70 6.0 6.2
Laboratory atmosphere
60.0 58.9 1.33 4 0.17 41.9 0.05–0.50 13 7.6 8.0
58.9 1.33 8 0.45 43.5 0.10–0.50 28 7.0 8.2
58.9 1.33 16 1.07 43.6 0.10–2.00 66 6.9 8.7

Fig. 13. Photographs of cracks for different material thicknesses: (a) 4 mm; (b) 8 mm; (c) 16 mm. Samples were confined in hermetic
containers with a relative humidity of 75%; diameter of the container is 225 mm.

and in hermetic containers (closed system). The water loss
per unit area is higher in samples tested in the laboratory
than in those in the containers. According to this result, at
the time of the crack initiation, none of the samples attained
equilibrium. The linear relationship between water losses per
unit area versus time in the initial drying process is in agree-
ment with that from other works (Towner 1987a; Blight
1997; Rodríguez 2002b).
The initial dry density, under saturated conditions, affects the
shrinkage behaviour and water content when cracks appear
(Fig. 16). The cracks do not appear for water contents lower
than the retraction limit. When the sample is compacted to a
degree of saturation between 0.90 and 0.99, and the gravimetric
water content is superior to the retraction limit, cracks appear,
and the geometric characteristics and space distributions are
very different from those of the saturated condition. The desic-
cation cracks appear at the periphery of the sample.
Hydraulic conductivity
Saturated hydraulic conductivity, ksat, was measured by
imposing a constant-head gradient on a saturated specimen
placed in a permeameter cell. The results are plotted in
Fig. 17a, in which a clear dependence of ksat on the void ra-
tio, e, is highlighted. This relation is defined by the follow-
ing equation (see Aubertin et al. 1996):
[1] ksat = e y
where y is the material parameter.
For the ksat values measured and shown in Fig. 17a, the
value of y = 2.66, considering the material in solid and
slurry form (e = 3.6); when the value of e is low, however,
then y = 3.90.
Figure 17b presents the unsaturated hydraulic conductiv-
ity, kunsat, versus the degree of saturation measured during
the changes of suction imposed in the drying–wetting paths

© 2006 NRC Canada

Rodríguez 1055

Fig. 14. Results from desiccation tests: (a) distance between cracks versus waste thickness; (b) water content at crack initiation versus
prescribed suction; (c) time to crack initiation versus prescribed suction; (d) vertical strain versus prescribed suction. Solid symbols re-
fer to samples open to the laboratory atmosphere. h, material thickness.

used to define the retention curve shown in Fig. 10c. As ex-
pected, a large decrease in the permeability can be observed
when the material is unsaturated.
Figure 17c presents hydraulic conductivity versus hydraulic
gradients of between 3 and 25 for two different void ratios.
The hydraulic conductivity is constant for different hydraulic
gradients and different void ratios in homogeneous samples.
Effect of desiccation cracks on hydraulic conductivity
It has been observed that subsequent wetting and swelling
of the MW do not eliminate the discontinuities generated by
desiccation cracks, as occurs in clayey soils (Blight 1997).
This could be of a great importance for in situ hydraulic
conductivity under cyclic wetting and drying conditions. If a
certain degree of discontinuity remains in the MW even af-
ter sealing and mechanical confinement by the addition of
fresh MW, the hydraulic conductivity should reflect this ef-
fect. Saturated hydraulic conductivity, ksat, was measured by
imposing a constant-head gradient on a saturated specimen
placed in a triaxial cell under different confining stresses
(from 7 to 1500 kPa). Measurements of saturated hydraulic
conductivity were carried out on continuous samples and on

© 2006 NRC Canada

1056
Fig. 15. Rate of loss of water versus time for three different samples during the desiccation process in hermetically closed containers
(relative humidity = 65%, temperature T = 22 °C) and in the laboratory atmosphere (relative humidity = 65%, T = 22 °C).
Fig. 16. Relationship between initial gravimetric water content
and gravimetric water content at crack initiation and shrinkage.
layered and cracked samples (during 24 h). They are com-
pared in Fig. 15a, in which all measurements are shown as a
function of the sample void ratio. The continuous samples
were 120 mm in height and 100 mm in diameter, with an
initial dry density of 1.53 g/cm3. The layered samples were
prepared with layers of thicknesses H = 10 mm (12 layers),
Can. Geotech. J. Vol. 43, 2006
20 mm (6 layers), and 40 mm (3 layers) with the same initial
dry density. It should be pointed out that, according to
Fig. 15a, the effect of layering and crack formation in-
creases hydraulic conductivity. The value of saturated hy-
draulic conductivity depends on the initial void ratio and the
thickness of the layers. It is possible to increase the value of
saturated hydraulic conductivity between one to four orders
of magnitude in the samples with cracks compared with that
of the intact sample, depending on the initial dry density and
thickness of the layer. In all cases the relation between ksat
and the void ratio is defined by the equation ksat = ey. In this
case, the y value for homogeneous samples is similar to the
value obtained for hydraulic conductivity measured in the
permeameter test for a homogeneous sample with a similar
dry density (see Figs. 17, 18).
It is important to determine whether further addition of
material or further mechanical actions may close the cracks
and return the permeability to its original value (continuous
samples). Figure 15b shows that this is not the case for
these samples of MW, as isotropic stress confinement
of MW samples does not eliminate the presence of the dis-
continuities generated by previous desiccations. The results
were obtained for a continuous sample and for layered
specimens with different layer thicknesses (H), as previ-
ously indicated.
© 2006 NRC Canada
Rodríguez
Fig. 17. Relationship between (a) saturated hydraulic conductivity and waste void ratio, (b) degree of saturation and unsaturated hy-
draulic conductivity for void ratios (e) between 1.70 and 1.56, and (c) saturated hydraulic conductivity and hydraulic gradient for two
different void ratios (1.75 and 1.45).
The observed increase in hydraulic conductivity due to
cracking is in agreement with results reported for clayey
soils (Bronswijk 1988; Scanlon 1992; Drumm et al. 1997;
Jørgensen et al. 1998; Kelly and Pomes 1998). In particular,
the work of Jørgensen et al. (1998) presents laboratory infil-
tration tests where the effect of cracking on chloride and
pesticide transport is studied in three columns of clayey soil.
Jørgensen et al. observed that the hydraulic conductivity and
transport of contaminants are mainly controlled by fractures
that become preferential flow paths. This could also be the
case in the deposits considered in this paper, and future work
should take this effect into account.
Conclusions
From the experimental study, it can be concluded that the
ammoniacal ammonium carbonate leaching (ACL) metallur-
gical waste (MW) collected from a tailings impoundment in
Moa, Cuba, has a grain-size distribution similar to that of a
silt soil. It is formed by iron minerals and heavy metals. It
1057
presents low plasticity, a null cohesion, and a high friction
angle (36°). The material studied can be geotechnically clas-
sified as low-plasticity silt (ML). Results of undrained
triaxial tests on remoulded samples indicate a dilative be-
haviour, with a decrease in pore-water pressure near fail-
ure. MW is susceptible to liquefaction in the presence of a
cyclic load in triaxial tests. The void ratio decreases signifi-
cantly during the consolidation test and the drying process.
The relationship between the hydraulic conductivity and
void ratio is ksat = ey.
Hydraulic conductivity, soil stiffness, and compressive
and tensile strength of the MW have an important depend-
ence on the degree of saturation and vary significantly dur-
ing the drying process. In the range of MW thicknesses and
suctions used in the tests, the distance between cracks seems
to be related to thickness and not to the imposed suction. In
general, in a drying process applied to saturate MW, initia-
tion of cracks occurs under quasi-saturated conditions and
with a small increase in horizontal tensile stresses due to the
low tensile stiffness of the MW close to saturation.
© 2006 NRC Canada
1058
Fig. 18. Saturated hydraulic conductivity of the waste measured in continuous and layered samples as a function of (a) void ratio, and
(b) confining stress. H, thickness of the layers.
Unconfined compressive and tensile strengths gave maxi-
mum values for degrees of saturation (Sr) of about 0.8 and
0.9, respectively. These values correspond to suctions be-
tween 0.05 and 0.40 MPa in the water retention curve. Ap-
parently, desiccation cracks appear under similar conditions,
for Sr values between 0.8 and 0.9.
It has been observed that after desiccation-induced surface
cracking, subsequent wetting or crack filling with fresh MW
does not eliminate the original discontinuities. The hydraulic
conductivity measured in samples with cracks is one order
of magnitude higher than the value measured for continuous
homogeneous samples of MW. From an environmental point
of view, the hydraulic conductivity results for the desiccation
cracks have important implications in flow and transport
analyses on these MW deposits. These results may be useful
for other cases involving similar and poorly character-
ized MW.
Can. Geotech. J. Vol. 43, 2006
Acknowledgements
This work was done in the framework of the Spanish Na-
tional Project PPQ2001-2100-C04 and PB/44/FS/2002 fi-
nanced by Fundación Séneca, Murcia, Spain. The paper also
benefited from the constructive comments of two anony-
mous reviewers and the associated editor.
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