Minerals Engineering 134 (2019) 269–274

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Minerals Engineering
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Short communication

Improved understanding of chalcopyrite flotation in seawater using sodium T

hexametaphosphate
⁎
Wanqing Lia, Yubiao Lia,b,
a
School of Resources and Environmental Engineering, Wuhan University of Technology, Wuhan 430070, China
b
State Key Laboratory of Mineral Processing, BGRIMM Technology Group, Beijing 100160, China

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

Keywords: Due to the scarcity of freshwater, the application of seawater has been considered as an alternative in mineral
Chalcopyrite flotation. Previous studies reported that the challenges of using seawater was due to various ions contained, but
Flotation not many achievements in relieving their negative effects have been obtained. This study systematically in-
Seawater vestigated the application of sodium hexametaphosphate (SHMP) in chalcopyrite (CuFeS2) flotation in seawater,
SHMP
as well as in the presence of Mg2+ or Ca2+ (two divalent ions displayed the most significantly negative roles on
mineral flotation). It was found that the detrimental effects of seawater on CuFeS2 flotation were primarily due
to the formed Mg(OH)2 colloids (major) and CaCO3 precipitates (minor) attaching onto CuFeS2, giving rise to a
hydrophilic CuFeS2 surface. The presence of SHMP significantly increased CuFeS2 recovery in seawater and in
the solution containing Mg2+ and Ca2+. Two beneficial mechanisms due to SHMP were proposed. Firstly, SHMP
combined with Ca2+ and Mg2+ to form dissolvable complexes, reducing the formation of hydrophilic Ca and Mg
precipitation. Secondly, SHMP reversed the interaction force between CuFeS2 particles and Mg(OH)2 colloids
from attractive to repulsive, thereby reducing the attachment of these precipitates onto CuFeS2 surface. This
study therefore provides a promising way in utilizing seawater for mineral flotation.

1. Introduction
Seawater, with a 3.5 wt% salinity, comprises nearly 97% of the
earth’s water resources (Qiu et al., 2016; Wang and Peng, 2014). Due to
the freshwater shortage, the application of seawater in mineral flotation
has attracted increasing interests from both industrial community and
academic world (Wang and Peng, 2014). However, many inorganic ions
(e.g. K+, Na+, Ca2+, Mg2+, Cl−, and SO42−) contained in seawater are
capable of changing the frothing properties (e.g. frothing stability,
bubble coalescence) of pulp and the surface properties (e.g. hydro-
phobicity, electrostatic force) of minerals particles, further influencing
mineral floatability (Jeldres et al., 2016; Romero et al., 2018; Wang and
Peng, 2014).
Some studies reported that the seawater conditioned at alkaline
condition was detrimental to flotation process (Ikumapayi, 2016;
Jeldres et al., 2017; Jeldres et al., 2016; Ramos et al., 2013; Suyantara
et al., 2018). It is widely recognized that the hydrolysable Ca2+ and
Mg2+ in seawater can easily form metallic precipitation attaching on
mineral surface, thereby reducing flotation recovery (Hirajima et al.,
2016; Jeldres et al., 2017; Li et al., 2017b; Liu and Zhang, 2000;
Rebolledo et al., 2017). For instance, Wang and Peng (2014) reported
that saline water can modify hydration layer and electrical double
layers of mineral particles, as well as the bubble coalescence and sta-
bility. Although these studies have focused on the effects of salts on
mineral floatability, the reported results varied and even conflicted,
keeping underlying mechanisms unclear (Choi et al., 2016; Ikumapayi,
2016; Liu et al., 2013).
As chalcopyrite (CuFeS2) is the most abundant Cu-bearing mineral
(Li et al., 2013) and predominantly processed via flotation, much at-
tention has been paid to investigate the effects of seawater on its flo-
tation efficiency. Most studies have shown that CuFeS2 recovery was
significantly influenced due to the application of seawater, e.g.
Suyantara et al. (2016) found that CuFeS2 recovery was reduced due to
the adsorption of Mg(OH)2 precipitation, similar to that reported in
Hirajima et al. (2016). Although some mechanisms on how the ions
affecting CuFeS2 flotation have been proposed, less attention has been
paid to reduce the negative effects derived from seawater.
As a common dispersant, sodium hexametaphosphoate (SHMP) has
been widely used in industrial implementation, e.g. Xu et al. (2016)
reported that SHMP increased the electrostatic repulsion between va-
luable minerals and gangues, showing dispersing effect. Although Li
et al. (2018a) found that the presence of SHMP relieved the inhibition

⁎
Corresponding author.
E-mail address: Yubiao.Li@whut.edu.cn (Y. Li).

https://doi.org/10.1016/j.mineng.2019.02.019
Received 24 July 2018; Received in revised form 31 January 2019; Accepted 5 February 2019
Available online 11 February 2019
0892-6875/ © 2019 Elsevier Ltd. All rights reserved.
W. Li, Y. Li
of Ca2+ and Mg2+ on CuFeS2 recovery, the roles of SHMP on CuFeS2
flotation in the presence of Ca2+ and Mg2+ and seawater have not been
systematically investigated.
Therefore, SHMP was applied in this study to reveal its roles in
improving CuFeS2 flotation in seawater, 0.05 M Mg (referred to Mg
concentration in seawater) and 0.01 M Ca (referred to Ca concentration
in seawater), thereby providing new insights into the possibility of
using seawater or saline water for CuFeS2 flotation in the future.
2. Materials and methods
2.1. Materials
A pure CuFeS2 sample provided by Australia GEO discoveries was
used in this study, with the 38–75 µm powder particle being obtained
following the same procedure reported in Li et al. (2018a). China Si-
naopharm Chemical Reagent Co. (Shanghai, China) provided the fol-
lowing reagents (analytical grade), SHMP, NaOH, CaCl2 and
MgCl2·6H2O. Millipore® ultrapure water (Billerica, MA, USA) was used
as freshwater.
2.2. Flotation experiment
A XFGIItype flotation machine (Fig. 1) was used for flotation ex-
periment (XFG 5–35 g, Wuhan Exploration Machinery Factory, Wuhan,
China). 1 g of CuFeS2 powder (38–75 µm) was added into a 25 mL flo-
tation cell, followed by adjustment to pH 10 using NaOH within 5 min,
at a stirring speed of 1200 rpm. As entrainment is a nonselective process
transferring both gangue and valuable particles into the froth phase by
the rising bubbles, the particle size should be selected carefully for
flotation. Some previous studies such as (Neethling and Cilliers, 2002)
reported that 20 μm was the lower limit for entrainment phenomenon.
In addition, the particle size of 38–75 µm has been widely adopted in
published work (Fang et al., 2017; Lucay et al., 2015; Qiu et al., 2017).
Therefore, the entrainment phenomenon is not expected herein.
After 1.2 cm/s air was introduced, the froth was collected at 1, 3, 5,
8 and 10 min with a scraping rate of 10 s. Both the floated concentrate
and residue were air dried at 70 °C and then weighed to calculate flo-
tation recovery. The seawater was prepared according to the main
composition of seawater published in Qiu et al. (2016) and Suyantara
et al. (2018), including 0.47 M NaCl, 0.01 M KCl, 0.01 M CaCl2, 0.025 M
MgCl2, 0.0018 M NaHCO3, 0.028 M MgSO4, and 0.00087 M KBr. It
should be noted that no flotation reagents (collectors, frothers) were
using during flotation process as the natural floatability of chalcopyrite
is expected herein.
Fig. 1. XFG II type flotation machine.
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Minerals Engineering 134 (2019) 269–274
2.3. Species diagram
Species diagrams of seawater with a total ionic strength of 0.7 M in
a system open to air was calculated using Medusa software. The ion
concentration of seawater was referred to that in Qiu et al. (2016).
2.4. Contact angle measurements
Prior to contact angle measurements, the freshly polished CuFeS2
slab was treated in solution conditioned at pH 10 for 10 min, which was
then softly washed using ultrapure water and air dried. Subsequently, a
JC2000C type contact angle measuring device (Shanghai Zhongchen
Digital Technology Company, China) was used to take image and cal-
culate the contact angle following the sessile drop method (Goclawski
and Urbaniak-Domagala, 2007).
2.5. Froth layer measurements
The froth layer measurements were carried out in a glass froth
column (GA-61, Shanghai Silicone Industry Co. Ltd., Shanghai, China)
with a height of 70 cm and an internal diameter of 4 cm. Prior to
measurement, 100 mL of prepared pulp (2% solids) were poured into
the column. Thereafter, the compressed air with 0.88 cm/s was in-
troduced through the bottom of a glass sand filter. When the froth
height was stable, the formed froth layer height was recorded.
2.6. Zeta potential measurements
A Nano-ZS90 zeta potential analyzer (Malvern Co., Ltd, Malvern,
UK) was used to measure the zeta potential of CuFeS2. Suspensions
were prepared by adding 0.05 g of CuFeS2 (−5 µm) to 50 mL solution
and then magnetic stirred during the first 10 min, followed by adjusting
the pulp pH using NaOH solution. The final suspension was sampled for
zeta potential measurements. Each measurement was repeated at least
three times and the average of zeta potential were presented herein.
2.7. XPS measurements
XPS analyses were performed using ESCALAB 250Xi spectrometer
(Thermo Fisher Scientific Inc., MA, USA) with an Al Kα mono-
chromated X-ray source. The broad scans were collected from 1350 to
0 eV with a 100 eV pass energy, 1.0 eV step size and 0.1 s dwell time.
The spectra were calibrated by setting C 1s peak at 284.8 eV for cali-
bration. All XPS spectra were fitted using XPS Peak4.1 software.
3. Results and discussion
3.1. Flotation results
Fig. 2 shows a 76% CuFeS2 recovery at 10 min in the freshwater,
indicating a good natural floatability of CuFeS2. A sharp decrease to
36% was observed when seawater was applied, indicating negative
effects of seawater on CuFeS2 flotation, consistent with that found in
Suyantara et al. (2018). However, our results are different from that
observed in Castro et al. 2012, highly likely due to the differences in
pulp density and flotation reagents, e.g., Castro (2012) used a very high
pulp density (35 wt%) and flotation reagents (e.g., collectors and
frothers), while a relatively lower pulp density (4 wt%) in the absence
of any collector and frother was applied herein to investigate the nat-
ural floatability of chalcopyrite. Although a 55% CuFeS2 recovery was
observed in 0.01 M CaCl2 solution, only 12% CuFeS2 was recovered in
0.05 M MgCl2. These indicated that the depressing effects of seawater
was predominantly due to Mg2+.
In the presence of 50 mg/L SHMP, CuFeS2 recovery was influenced
to different extents. Although CuFeS2 recovery in freshwater was not
significantly affected, CuFeS2 recoveries in seawater, 0.05 M MgCl2 and
W. Li, Y. Li
Fig. 2. CuFeS2 recovery at pH 10 with and without 50 mg/L SHMP.
0.01 M CaCl2 solution were increased, indicating that SHMP was cap-
able of relieving the negative effects due to the presence of major di-
valent ions. It should be noted that the increase in CuFeS2 recovery for
both seawater (from 36% to 88%) and MgCl2 (from 12% to 64%) were
52% while only a 7% increase in CuFeS2 recovery was observed in
CaCl2 solution (from 55% to 62%). These suggested that the beneficial
roles of SHMP on CuFeS2 flotation in seawater was primarily due to the
reduced detrimental effects from Mg2+.
3.2. Contact angle
Fig. 3 shows a contact angle of 62° for fresh CuFeS2 surface treated
at pH 10 solution, indicating a high hydrophobicity of natural CuFeS2.
However, the presence of seawater, MgCl2 and CaCl2 reduced the
contact angle of CuFeS2 to 26°, 25° and 51°, respectively, consistent
with the declined CuFeS2 recovery shown in Fig. 2. When 50 mg/L
SHMP was added into solution, the contact angle of CuFeS2 treated in
freshwater was almost remained at the same level, suggesting that
SHMP had a negligible effect on CuFeS2 hydrophobicity in the absence
of ions. A slightly increased contact angle to 55° was observed in 0.01 M
CaCl2, indicating that SHMP played a weak benefit to relieve the de-
pression effects from Ca2+. However, much more significant increase
(approximately 30°) in contact angle was observed in both seawater and
0.05 M MgCl2 solution, agree well with CuFeS2 flotation results.
Fig. 3. Contact angle of CuFeS2 treated in various solutions at pH 10.
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Minerals Engineering 134 (2019) 269–274
Table 1
Zeta potential (mV) of CuFeS2 in various solutions at pH 10.
SHMP Freshwater Seawater 0.05 M MgCl2 0.01 M CaCl2
0 −42.1 20.7 28.5 5.1
50 mg/L −70.3 −18.6 −11.8 −21.4
3.3. Zeta potential
Table 1 shows the zeta potential of CuFeS2 treated in various solu-
tions at pH 10. A negative charge of −42.1 mV was observed for fresh
CuFeS2, which was however increased to positive values in seawater or
MgCl2/CaCl2 solution, probably due to the adsorption of positively
charge metallic species (e.g. Mg(OH)2 precipitation) on negatively
charged CuFeS2 surface (Li et al., 2018a).
The addition of SHMP led to a more negative zeta potential
(−70.3 mV) in freshwater while the zeta potentials of CuFeS2 in sea-
water or MgCl2/CaCl2 solution were reversed from positive to negative
values. It should be noted that the change in zeta potential of MgCl2 and
seawater was the same (i.e. decreased 39.3 mV), further indicating that
the roles of SHMP on seawater was mainly on MgCl2. As indicated in
previous studies (Hirajima et al., 2016; Jeldres et al., 2017; Li et al.,
2017b; Liu and Zhang, 2000; Rebolledo et al., 2017), the presence of
MgCl2 produced Mg precipitation (e.g. Mg(OH)2) that adsorbed on
mineral surface, thereby decreasing CuFeS2 recovery. Therefore, the
beneficial role of SHMP is likely due to the inhabitation of metallic
precipitation adsorption on CuFeS2 surface.
3.4. Froth layer thickness measurements
Generally, the froth layer thickness responds to the frothing ability
of pulp. An increase in froth ability refers to increased bubble-particle
attachments, further improving mineral recovery (Farrokhpay, 2011).
As shown in Fig. 4, the froth layer thickness was apparently greater in
seawater compared to freshwater, revealing a stronger frothing ability
due to seawater. Similar phenomenon was observed by Ramos et al.
(2013) who found that the froth layer thickness of Cu-Mo ores in sea-
water was higher than that in freshwater. However, the froth layer
thickness in divalent solutions was similar to that in freshwater in the
absence of SHMP, indicating Ca2+ and Mg2+ in seawater were not the
main reason for high frothing ability of seawater. Previous studies
(Castro et al., 2013; Wang and Peng, 2014) showed that high NaCl
concentration can increase the frothing ability of solution. Li et al.
(2017a) found an increased froth layer height when NaCl concentration
was increased to 0.5 M (closed to 0.47 M present in seawater).
Fig. 4. Froth layer thicknesses in various solutions at pH 10.
W. Li, Y. Li
Fig. 5. Mg and Ca species diagram of seawater.
Therefore, the higher CuFeS2 recovery in seawater than that in MgCl2
solution (Fig. 2) was likely due to stronger frothing ability from other
ions (e.g. Na) in seawater.
It should also be noted that the addition of SHMP slightly decreased
the froth layer thickness in all solutions, indicating that SHMP was
detrimental to the frothing ability of the solution. Although this oc-
curred, CuFeS2 recovery was still increased in the presence of SHMP
(Fig. 2), indicating that the beneficial roles due to SHMP overcame its
detrimental effects in frothing ability. The beneficial roles will be dis-
cussed in Section 3.7 in detail.
3.5. Speciation calculation
Fig. 5 shows the distribution of Mg and Ca species in seawater.
Within the pH range investigated, Ca carbonate precipitation (Ca-
CO3(cr)) and Mg hydroxide precipitation (Mg(OH)2(cr)) were formed at
pH greater than 7.6 and 9.5, respectively. When pH was 10 (flotation
pH herein), only 2.0 mM CaCO3(cr) was formed in the solution, sig-
nificantly lower than that of Mg(OH)2(cr) (46 mM). Therefore, decreased
CuFeS2 recovery in seawater can be due to the adsorption of Mg
(OH)2(cr) (major) and CaCO3(cr) (minor) on CuFeS2 surface.
3.6. XPS analysis
Fig. 6 shows the XPS survey spectra of CuFeS2. No Mg 1s or Ca 2p
peaks were found on the untreated CuFeS2 surface (Fig. 6(a)). However,
Fig. 6. XPS survey spectra of CuFeS2, (a) untreated, treated in (b) seawater and
(c) seawater + SHMP.
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Table 2
Elemental quantification (at %) of CuFeS2 surface.
Element BE (eV) Conditions
Untreated Seawater Seawater + SHMP
C 1s 284.8 18 31 27
S 2p 161.5 27 17 23
O 1s 532.1 19 26 21
Fe 2p 710.8 16 8 11
Cu 2p 932.6 19 11 15
Ca 2p 352.0 0 2 1
Mg 2s 1304.7 1 5 2
Noted: All BE with a typical variation of ± 0.2 eV.
O 1s peak was present on the untreated chalcopyrite surface, indicating
that this chalcopyrite sample experienced oxidation to some extents.
The oxidation of chalcopyrite in air or in solution has been reported in
many previous studies due to the readily oxidation properties of chal-
copyrite (Li et al., 2017c; Li et al., 2018b; Wei et al., 2016). Once
treated in seawater (Fig. 6(b)), both Mg 1s and Ca 2p peaks appeared.
As indicated in Fig. 5, Mg(OH)2(cr) and CaCO3(cr) can be formed on
CuFeS2 surface, the increased O 1s (Fig. 6(b)) might be due to the ad-
sorption of these two species on CuFeS2 surface. However, when 50 mg/
L SHMP was added, the peak intensities of Mg 1s, Ca 2p, O 1s and C 1s
were decreased significantly, illustrating that SHMP reduced the ad-
sorption of Mg(OH)2(cr) and CaCO3(cr) on CuFeS2 surface.
The detailed elemental composition of CuFeS2 surface is presented
in Table 2. As compared to the untreated CuFeS2 surface, significant
increases in Mg, Ca, C and O were observed, i.e. from 1% to 5%, 0% to
2%, 18% to 31%, and 19% to 26%, respectively, which however were
decreased to 2%, 1%, 27% and 21%, respectively when SHMP was
applied. These suggested that the application of seawater increased Mg,
Ca, C and O concentrations on CuFeS2 surface, which can be attributed
to the adsorption of Mg(OH)2(cr) and CaCO3(cr). Accordingly, SHMP can
reduce the adsorption of Mg(OH)2(cr) and CaCO3(cr) on CuFeS2 surface.
3.7. Mechanisms
Previous studies showed that SHMP had a complexing ability with
ions such as Ca2+ and Mg2+ to form dissoluble complexes (Li et al.,
2018a; Rebolledo et al., 2017). The SHMP added in this study was only
0.08 mM, which was not able to complex these precipitations formed in
seawater at pH 10 (e.g. 2.0 mM CaCO3(cr) and 46 mM Mg(OH)2(cr),
Fig. 5). Therefore, the complexing mechanism of SHMP was not pri-
mary to the improved CuFeS2 recovery.
The results discussed above suggested that the negative effects of
seawater on CuFeS2 flotation was primarily due to the divalent ion of
Mg2+, rather than Ca2+. Therefore, the beneficial roles of SHMP will be
focused on Mg2+. As SHMP is normally considered as a dispersant, the
interaction energies between CuFeS2 particles and Mg(OH)2 colloids
with and without SHMP were investigated basing on EDLVO theory.
Fig. 7(a) showed a negative Van der Waals interaction energy (VW) and
a more negative electrostatic interaction energy (VE) within all particle
distances examined, giving rise to a negatively total interaction energy
(VT) between CuFeS2 and Mg(OH)2. Therefore, the aggregation be-
tween CuFeS2 and Mg(OH)2 colloids was dominated by attraction force.
It should also be noted that the absolute value of VE was apparently
greater than that of VW, indicating that the negative VE played a pri-
mary role between CuFeS2 particles and Mg(OH)2 colloids.
Fig. 7(b) showed that the addition of SHMP resulted in steric hin-
drance interaction energy (VSR) due to the steric hindrance effects (Lu
et al., 2011; Wang et al., 2007). The absolute value of VSR was the
greatest within the particle distance range, suggesting that the positive
VSR dominated the force between CuFeS2 and Mg(OH)2 colloids. In
addition, the reverse of VT from negative (without SHMP, Fig. 7(a)) to
W. Li, Y. Li
Fig. 7. Interaction energy between CuFeS2 particles and Mg(OH)2 colloids.
positive (with SHMP, Fig. 7(b)) values, indicating that the repulsion
force dominated. Therefore, the increased CuFeS2 recovery in the pre-
sence of SHMP was mainly due to the prevention of hydrophilic Mg
(OH)2 attaching onto CuFeS2 surface.
4. Conclusions
Reduced CuFeS2 recovery was observed in the presence of Mg2+,
Ca2+ and seawater due to the formed hydrophilic Mg(OH)2(cr) or
CaCO3(cr) adsorbed onto CuFeS2 surface. The detrimental effects of
seawater on CuFeS2 flotation were found to be primarily from the
presence of Mg2+, rather than Ca2+. EDLVO theory indicated that a
very strong electrostatic attraction force was presented between CuFeS2
particles and Mg(OH)2 colloids, resulting in an interparticle aggrega-
tion and a hydrophilic CuFeS2 surface.
The addition of SHMP significantly improved CuFeS2 recovery in
seawater, mainly due to two mechanisms. The primary mechanism was
the reverse of interaction force between CuFeS2 particles and Mg(OH)2
colloids from attraction force to repulsion force due to the strong steric
hindrance effects derived from SHMP. The repulsion force prevented
the attachment of hydrophilic Mg(OH)2 colloids formed onto CuFeS2
surface during flotation controlled at pH 10. Secondly, SHMP was
capable of complexing with Ca2+ and Mg2+ to form dissolvable com-
plexes, thereby reducing the formation of hydrophilic precipitation.
However, this mechanism plays a much less significant role on in-
creasing chalcopyrite flotation recovery due to the limited amount of
SHMP added during flotation process. In other words, the roles of
SHMP in improving CuFeS2 flotation recovery in seawater was pri-
marily achieved by reducing the adsorption of Mg species onto its
surface and decreased its wettability.
Acknowledgements
This project is financially supported by the National Natural Science
Foundation of China (51604205, 51774223) and Natural Science
Foundation of Hubei Province (2016CFB268). The authors also grate-
fully acknowledge the supports from Open Foundation of State Key
Laboratory of Mineral Processing (BGRIMM-KJSKL-2019-11) and
Fundamental Research Funds for the Central Universities (WUT:
2016IVA046 and 2017IVB018). A special thank is given to the financial
support for the Excellent Dissertation Cultivation Fund of Wuhan
University of Technology (2017-YS-052).
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Minerals Engineering 134 (2019) 269–274
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