Journal of Hazardous Materials 179 (2010) 940946

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Journal of Hazardous Materials

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

Utilization of water-reducing admixtures in cemented paste backll of

sulphide-rich mill tailings
Bayram Ercikdi , Ferdi Cihangir, Ayhan Kesimal, Haci Deveci, Ibrahim Alp
Department of Mining Eng., Karadeniz Technical University, 61080, Trabzon, Turkey

a r t i c l e i n f o a b s t r a c t

Article history: This study presents the effect of three different water-reducing admixtures (WRAs) on the rheological
Received 1 March 2010 and mechanical properties of cemented paste backll (CPB) samples. A 28-day strength of 0.7 MPa and
Received in revised form 23 March 2010 the maintenance of the stability (i.e. 0.7 MPa) over 360 days of curing were desired as the design criteria.
Accepted 23 March 2010
Ordinary Portland cement (OPC) and Portland composite cement (PCC) were used as binders at 5 wt.%
Available online 27 March 2010
dose. WRAs were initially tested to determine the dosage of a WRA for a required consistency of 7
for CPB mixtures. A total of 192 CPB samples were then prepared using WRAs. The utilization of WRAs
Keywords:
enhanced the ow characteristics of the CPB mixture and allowed to achieve the same consistency at a
Cemented paste backll
Water-reducing admixtures
lower water-to-cement ratio. For OPC, the addition of WRAs appeared to improve the both short- and
Sulphide tailings long-term performance of CPB samples. However, only polycarboxylate-based superplasticiser produced
Consistency the desired 28-day strength of 0.7 MPa when PCC was used as the binder. These ndings suggest that
Stability WRAs can be suitably exploited for CPB of sulphide-rich tailings to improve the strength and stability in
short and long terms allowing to reduce binder costs in a CPB plant.
2010 Elsevier B.V. All rights reserved.

1. Introduction In concrete industry, water-reducing admixtures (WRAs), also

Process tailings mixed with water and a hydraulic binder can
be placed underground as cemented paste backll (CPB) [1]. CPB
is potentially one of the best practical approaches for the manage-
ment of process tailings since it offers signicant environmental,
technical and economic benets. These include the alleviation of
the environmental impact of potentially hazardous mill tailings
(e.g. sulphide tailings, in particular) by disposal of them safely into
underground, the support of underground openings to provide a
safe working environment and minimize surface subsidence, and
the reduction of the tailings disposal and rehabilitation costs [24].
The amount of the tailings to be placed underground depend on the
solids contents (typically ranges between 70 and 85 wt.% solids) and
owability of the paste mixtures. Increasing solid concentration
usually increases the strength and stability of CPB at the expense
of a reduction in the consistency (slump) of mixtures. It is of prac-
tical importance to note that CPB is required to contain sufcient
water to achieve the desired consistency for its transport from the
paste plant to the underground openings. However, an increase in
the water-to-cement (w/c) ratio adversely affects the strength and
stability of CPB [5].
Corresponding author at: Karadeniz Teknik Univ. Maden Muh. Bol. 61080, Tra-
bzon, Turkey. Tel.: +90 462 377 3171; fax: +90 462 325 7405.
E-mail address: bercikdi@ktu.edu.tr (B. Ercikdi).
known as plasticisers and superplasticisers, are extensively used
to produce high strength concrete without increasing the dosage
of a binder [69]. Lignosulphonate, naphthalene sulfonate and
polycarboxylate-based admixtures are the well-known reagents
with their capacity to reduce water content by 530% [710].
Papayianni et al. [8] reported that the concrete mixtures containing
a polycarboxylate type WRA produced 1.5 times higher UCSs than
those of reference mixtures at 28 days of curing period. Erdogdu
[7] demonstrated that the impact of a superplasticiser depended
on the cement type with the highest gain of strength that occurred
at a dosage of 3% of dry cement.
WRAs could be potentially exploited for CPB since the desired
consistency for the transport of CPB to underground can be
achieved at low w/c ratios with the likely reduction in the oper-
ational costs of CBP [1113]. The reduction in w/c ratio would be
expected to improve microstructure and alleviate the short- and
long-term strength and stability problems encountered particu-
larly in CPB of sulphide-rich tailings [5]. These problems are alleged
to be associated with the oxidation of pyrite present in the tailings
[1419]. Despite extensive use in concrete, the use of WRAs in CPB
has received very limited attention with no data available on CPB
of high sulphide tailings. Klein and Simon [12] reported the bene-
cial effect of WRAs on the strength and stability of CPB samples
prepared from low grade sulphide tailings (5.9%S). They recorded
consistently higher UCSs (1.8 times over 360 days) than those of CPB
without WRA presumably due to the reduction of water content
from 28% to 2426%.

0304-3894/$ see front matter 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.jhazmat.2010.03.096
 B. Ercikdi et al. / Journal of Hazardous Materials 179 (2010) 940946 941

Table 1
Chemical and physical properties of binders and tailings used [5].

Oxide composition SiO2 (%) Al2 O3 (%) Fe2 O3 (%) CaO (%) MgO (%) Na2 O (%) K2 O (%) S (%) Remarks

Tailings 11.39 3.27 50.9 0.95 1.19 0.17 0.23 26.2 49% FeS2
OPC 20.3 5.9 2.8 61.0 1.2 0.3 1.1
PCC 24.51 7.15 3.42 54.36 1.24 0.53 1.38 20% additive

Physical properties Gs () SS (cm2 /g) >90 m (%) >45 m (%) D10 (m) D30 (m) D80 (m) Cu (m) Cc () %Fine
(<20 m)

Tailings 4.09 3584 4.0 15.0 62 9.3 1.52 40

OPC 3.01 4345 2.2 15.8
PCC 2.94 4280 2.1 15.4

Gs : specic gravity; SS : specic surface; Cu : coefcient of uniformity (D60 /D10 ); Cc : coefcient of curvature ((D30 )2 /(D10 D60 )).

Table 2
Properties of the WRAs used in the tests.

P1 SP1 SP2

Commercial name EUCO-FILL 30 (Euclid Chemical Inc.) IKSAMENT NS (Iksa Beton ve POLYCAR-100 (Iksa Beton ve
Yap Kimyasallar Inc.) Yap Kimyasallar Inc.)
Chemical base Lignin Poly naphthalene sulfonate Polycarboxylate condensate
condensate
Recommended dosage (%by mass of cement) 0.50.7 1.01.2 1.51.8
Standard (ASTM C 494) Type A Type F Type F
Density (g/cm3 ) 1.19 1.22 1.05
pH 6.69.6 6.58.0 6.58.0

In this study, the effect of three different WRAs on the rheologi-
cal properties of CPB mixtures produced from sulphide-rich tailings
was examined using ordinary Portland cement and Portland com-
posite cement as binders. The inuence of WRAs on the strength
and stability performance of CPB was also evaluated over a cur-
ing period of 360 days. Potential benets of WRAs for CPB were
discussed.
2. Materials and methods
2.1. Tailings and binders
The tailings sample used in this study were obtained from a
copperzinc underground mine located in the northeast of Turkey.
Particle size analysis of the tailings indicated that the tailings can
be classied as a medium size tailings material since 40 wt.% of the
sample was ner than 20 m in size (Table 1) [20]. Chemical com-
position of the tailings and binders were performed according to
TS EN 196-2 [21]. The tailings sample was determined to be rich
in sulphide (26.2% S) (Table 1) and to contain pyrite as the major
sulphide mineral [5]. Further detailed physical, chemical and min-
eralogical properties of the tailings used in this study can be found
elsewhere [5,22,23]. Ordinary Portland cement (OPC) (Type I) and
Portland composite cement (PCC) were used as the binders in this
study (Table 1). PCC contains a natural pozzolan of volcanic origin
(14%) and limestone (6%) as mineral admixtures.
2.2. Admixtures
Three different water-reducing admixtures (P1, SP1 and SP2)
were used as the WRAs in this study. P1 is a lignin sulphonic
based agent composed of water, calcium lignosulfonate, sodium
lignosulfonate and triethanolamine. SP1, namely polynaphthalene
sulfonate condensate, and SP2, namely polycarboxylate conden-
sate, are particularly suggested for the applications where high
range water reducing and high performance for strength are
desired [8]. These admixtures (Table 2) comply with the relative
specications in ASTM C 494 [24].
2.3. Slump tests
A series of slump tests were performed to evaluate the consis-
tency of CPB mixtures to achieve 7 slump. WRAs were tested by

Table 3
A summary of the experimental conditions used in the preparation of CPB samples.

Binder type Additive type and dosage Solids content (SC)b (wt.%) Binder dosage (BD)c (wt.%) Water-to-cement ratio (w/c)d Slump (in.)
a
Type AD (wt.%)

OPC 77.0 5.0 5.97 7.0

P1 7.0 78.1 5.60 7.2
SP1 6.0 78.2 5.59
SP2 5.4 5.58

PCC 77.0 5.0 5.97 7.0

P1 7.0 78.1 5.60
SP1 6.0 78.2 5.59
SP2 5.4 5.58
a 100(MWRAs )
AD : (Mdry-binder )
.
b 100(Mdry-tailings +Mdry-binder )
SC : (Mdry-tailings +Mdry-binder +Mwater +MWRAs
.
c 100(Mdry-binder )
BD : (Mdry-binder +Mdry-tailings)
.
d Mwater +MWRAs
w/c : Mdry-binder
; (M: weight).
942 B. Ercikdi et al. / Journal of Hazardous Materials 179 (2010) 940946
Fig. 1. Preparation and testing of CPB samples: mixing (a); casting (b); curing (c) and UCS tests (d).
varying their dosages in the range of 0.77.0% (i.e. by mass of dry
binder). Binder dosage was kept constant at 5 wt.% of solids (tailings
plus binder on dry basis). Previous studies have shown that WRAs
are more effective when their addition to the paste is delayed by
3060 s after the cement comes into contact with water [12,25].
Therefore, the WRAs were added in 1 min after the cement come
into contact with water. The slump tests were conducted according
to ASTM C 143 [26].
2.4. Preparation and testing of CPB samples
A number of CPB samples (192 in total) were prepared by blend-
ing the tailings sample, binder (OPC and PCC), mix water (the
tailings water and tap water) and water-reducing admixtures in a
Univex SRMF20 Stand model blender equipped with a double spi-
Fig. 2. The effect of WRAs on the rheological properties of CPB samples prepared
from OPC and PCC at a binder dosage of 5 wt.%.
ral. The experimental conditions (i.e. w/c ratio, solids content and
slump) were given in Table 3.
The CPB mixtures were thoroughly mixed and poured into plas-
tic cylinders of 10 20 cm (D H cm) in size (Fig. 1a and b). The
open-top cylinders were placed in a humidity room for curing
(Fig. 1c). Over the curing period, the room was maintained at
approximately 80% humidity and 25 C temperature in order to
ensure the curing of the samples under the conditions similar to
the underground mines. Following a predetermined period (up to
360 days) of curing, the CPB samples were tested for unconned
compressive strength (UCS) according to ASTM C 39 [27]. Prior to a
UCS test, the ends of a sample were rectied to get plane surfaces.
UCS tests were performed using a computer-controlled mechanical
press, which had a load capacity of 50 kN and a displacement speed
of 0.5 mm per minute (Fig. 1d). The CPB systems are often designed
to produce a 28-day unconned compressive strength of 0.72 MPa
depending on the application [1]. In this study, the strength and
Fig. 3. The effect of WRAs on the mechanical performance of CPB samples prepared
from OPC at a binder dosage of 5 wt.%.
 B. Ercikdi et al. / Journal of Hazardous Materials 179 (2010) 940946
Fig. 4. The effect of WRAs on the mechanical performance of CPB samples prepared
from PCC at a binder dosage of 5 wt.%.
stability performance of CPB samples were evaluated based on the
threshold value of 0.7 MPa for 28-day UCS.
2.5. SEM and XRD studies
The fractured samples obtained from UCS tests after 360 days
were examined under a LEO Scanning Electron Microscope (SEM)
coupled with a Energy Dispersive Spectrometry (EDS) unit. The
samples were dried in an oven maintained at 50 C and then treated
with acetone to halt further hydration prior to SEM observations.
X-ray diffraction (XRD) (Philips Xpert PW 3040 Diffractometer)
analyses of the acetone-treated CPB samples were also performed
to examine the mineralogical composition of CPB samples after the
curing process. XRD scanning of the samples was carried out over
a 2 range of 570 with a 0.005 step size.
Fig. 5. SEM images of the CPB samples prepared from OPC+P1 (a) and OPC+SP2 (b) at a binder dosage of 5 wt.%.
943
Fig. 6. XRD pattern for the CPB sample prepared from PCC+ SP1 after a curing period
of 360 days (Py (Pyrite); Qtz (Quartz), Ill (Illite), Chl (Chlorite), C (Plaster of Paris),
Fsp (Feldspar), Brt (Barite)).
3. Results and discussion
3.1. Effect of water-reducing admixtures on the rheological
properties of CPB
The effect of WRAs on the rheological properties of cement-
based mixtures has been highlighted in many studies [8,9,11,28]. In
this study, the slump tests were initially designed to determine the
dosage of a WRA to produce a CPB mixture at 7 slump, which is the
minimum slump required for the efcient transport of CPB mixture
to underground as indicated by the plant practice [29]. Fig. 2 illus-
trates the effect of dosage of three different WRAs (P1, SP1 and SP2)
on the slump of CPB samples prepared from OPC and PCC at a xed
944 B. Ercikdi et al. / Journal of Hazardous Materials 179 (2010) 940946

binder dosage of 5 wt.%. As expected, the consistency of CPB mix-
tures increased with increasing the dosage of WRAs. The ndings
suggest that, compared with the control (i.e. no WRA), the water
content (and hence w/c ratio) of CPB mixtures at 7 slump could
be reduced by 6.6% by the addition of P1, SP1 and SP2 at those
predetermined dosages of, respectively, 7%, 6% and 5.4% (by mass
of dry binder).
The performance of WRAs appeared to depend on the binder
type as they are more effective for OPC than for PCC. The ndings
also showed the respective capacity of WRAs (i.e. P1, SP1 and SP2
in a decreasing order) based on the dosage required to produce a
7 slump. To illustrate, the required dosages of P1, SP1 and SP2 to
achieve 7 in. slump for CPB mixtures prepared from PCC were found
to be 7%, 6% and 5.4% (by mass of dry binder), respectively (Table 3).
CBP samples at 7 slump were shown to be produced at lower
dosages of these WRAs when OPC was used as the binder (Fig. 2).
Such variations in the performance of WRAa could be attributed
to inherent characteristics of binders, admixtures and interaction

Fig. 7. Visual appearance of 360-day cured CPB samples prepared from OPC without (a and c) and with WRA (b) showing the contribution of WRA to the stability of CPB as
indicated by the formation of no cracks.
 B. Ercikdi et al. / Journal of Hazardous Materials 179 (2010) 940946
between cement and admixtures [5,28]. Consistent with these nd-
ings, Erdogdu [7] also identied the composition of cement to be the
most inuential factor determining the mechanical performance
of a superplasticiser with its higher compatibility with OPC than
with PCCs. Huynh et al. [11] demonstrated the benecial effect of
polyphosphate and naphthalene sulfonate formaldehyde conden-
sate on the rheological properties (i.e. yield stress) of dewatered
tailings containing predominantly magnetite and quartz. They also
noted unexpectedly low performance for polyphosphate in CPB,
which was attributed to its chemical interaction with Ca in cement
phase.
3.2. Effect of water-reducing admixtures on the mechanical
properties of CPB
A previous study by the authors [5] had shown that CPB sam-
ples produced from the same tailings (Table 1) suffered consistently
from low strength and stability performance (i.e. failure to maintain
a UCS of 0.7 MPa over 28360 days of curing period) irrespec-
tive of the binder type (OPC, PCC and sulphate resistant cement) at
5% binder dosage. They had demonstrated that an increase in the
binder dosage (>5%) was required to achieve the desired mechan-
ical performance. They had also revealed that a reduction in w/c
ratio from 5.97 to 5.81 could remarkably ameliorate the strength of
CPB samples. However, it would have adversely affected the owa-
bility of CPB mixture as indicated by the corresponding decrease
in slump from 7 to 6.5 . Therefore, in the current study, WRAs
were tested to reduce w/c ratio and improve the owability and
strength performance of CPB without increasing binder dosage or
decreasing the slump value.
Figs. 3 and 4 show the effect of WRAs (P1, SP1 and SP2) on the
short- and long-term strength development of CPB samples pre-
pared from OPC and PCC at a xed binder dosage of 5 wt.%. In these
tests, P1, SP1 and SP2 were added at the predetermined dosages
for 7 slump (Fig. 2). The strength development of CPB samples
was similar in character in that the UCSs of CPB samples peaked
at an initial curing period of 56-90 days; thereafter, a tendency for
decline was observed.
The addition of WRAs was found to signicantly improve the
strength gain of CPB samples over the curing periods. The contri-
bution of WRAs to the mechanical performance of CPB depended on
type of agent and binder. In this regard, the superplasticisers (SP1
and SP2) were more effective than the plasticiser (P1) and, in terms
of strength gain, SP1 and SP2 were the most compatible WRAs
with OPC and PCC, respectively. Klein and Simon [12] tested the
performance of polycarboxylated acrylic acid-, naphthalene and
melamine sulfonic acid-based four different superplasticizers for
CPB of low sulphide (5.9% S) tailings. They observed that all the
WRAs improved the owability and 28-day strength of CPB and
allowed to reduce the water content from 28% down to 2426%.
They also noted that the carboxylated acrylic acid-based superplas-
ticizer was the most efcient leading to 80% higher one-year UCS
than that of the control.
The CPB samples prepared from OPC and WRAs were able to
produce a 28-day UCS of 0.7 MPa (i.e. the desired threshold value
for the mechanical performance) and to maintain the stability
(0.7 MPa UCS) over 360 days of curing periods. However, apart
from those containing SP2, PCC based CPB samples failed to develop
a UCS of 0.7 MPa at 28 days. Over the curing period between 90
and 360 days, the UCSs of CPB samples prepared from OPC and PCC
with WRAs were approximately 2050% higher than those of CPB
samples without WRAs. The addition of WRAs remarkably miti-
gated the deterioration in the stability of CPB samples of OPC and
PCC, i.e. only 18% and 13% losses in strength, respectively, cf. 25%
and 15% without WRAs over the same curing period. The benecial
effect of the addition of P1, SP1 and SP2 on the strength and sta-
945
bility CPB could be attributed to a better dispersion of the cement
and tailings grains in the CPB matrix and, more importantly, the
reduction of w/c ratio [9]. The microstructure of CPB is expected to
improve by the reduction in w/c ratio due to the decreased porosity
and permeability and hence, better particle packing and a denser
structure [5,8,11,30,31]. This may, in turn, mitigate the oxidation
of pyrite present in CPB due to the likely attenuation of ingress of
moisture and air.
It has been reported that sulphates (SO4 2 ) present in the mix-
ing water and those produced by the oxidation of pyrite present
in CPB can react with free calcium hydroxide (Ca(OH)2 ), giv-
ing rise to the formation secondary gypsum (CaSO4 2H2 O) and
ettringite (3CaSO4 Al2 O3 32H2 O) [5,1519,3234]. SEM and EDX
analysis of CPB samples indicated the presence of sulphate phases
(e.g. secondary gypsum and ferrous sulphate) within CPB sam-
ples with WRAs as shown in Fig. 5. No ettringite/gypsum was
identied in XRD studies of CPB samples with WRAs (Fig. 6) pre-
sumable due to their presence below the detection limit or low
crystallinity. The excessive formation of these expansive prod-
ucts can reduce the strength and stability of CPB as observed in
Figs. 3 and 4. In this regard, the development of severe cracks
was observed in the CPB samples without WRAs (Fig. 7a and
c). Consistent with their better mechanical performance, no such
cracks were apparent when WRAs were added (Fig. 7b). It is
pertinent to note that the formation of secondary gypsum or fer-
rous sulphate in certain quantity could be benecial allegedly
for lling the voids within CPB and, in turn, decreasing porosity
[32,35,36].
4. Conclusion
This study reveals the inuence of the addition of lignin
(P1), polynapthalene sulfonate (SP1) and polycarboxylate (SP2)
based water-reducing admixtures (WRAs) on the rheological and
mechanical properties of CPB produced from sulphide-rich tailings.
The addition of these WRAs appeared to improve the consistency
and the strength development of CPB. The performance of a WRA
depended mainly on the type of WRA and binder. Compared with
P1 and SP1, SP2 was the most effective agent producing the desired
slump of 7 at the lowest dosage. At the predetermined dosages
for 7 slump, WRAs allowed to reduce the water content (and
hence the w/c ratio) by 6.6% with the concomitant enhancement
(by 2050%) in the mechanical performance of CPB. OPC-based
CPB samples were able to achieve the desired mechanical perfor-
mance (i.e. 0.7 MPa UCS over 28 days) only in the presence of
WRAs. Furthermore, the addition of WRAs was shown to remark-
ably alleviate the stability problems (i.e. loss of strength) in the
long term. Despite the signicant improvement observed in the
strength development of PCC based CPB samples, the benecial
effect of WRAs on the long-term stability was limited and only those
samples containing SP2 produced the desired 28-day strength of
0.7 MPa.
This study highlights the benecial effect of WRAs in CPB of high
sulphide tailings to sustain/enhance the mechanical performance
and owability by reducing w/c ratio without increasing binder
dosage or decreasing the slump value.
Acknowledgements
The authors would like to express their sincere thanks and
appreciation for the nancial support to the Research Foundation
of Karadeniz Technical University (Project No: 2005.112.008.1),
to TUBITAK (The Scientic and Technological Research Council
of Turkey) (Project No: 107M183) and nally, to Prof. Dr. Sakir
Erdogdu for helping to improve the quality of the manuscript.
946 B. Ercikdi et al. / Journal of Hazardous Materials 179 (2010) 940946
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