Int. J. Miner. Process.

82 (2007) 148 155

www.elsevier.com/locate/ijminpro

Galvanic interactions between galenasphalerite and their reactivity

G. Urbano a , A.M. Melndez b , V.E. Reyes a,, M.A. Veloz a , I. Gonzlez b
a
rea Acadmica de Materiales y Metalurgia, Universidad Autnoma del Estado de Hidalgo,
Carr. Pachuca-Tulancingo KM 4.5, 42184 Pachuca, Hidalgo, Mexico
b
Departamento de Qumica, Universidad Autnoma Metropolitana Iztapalapa, 09340 Mxico D.F., Mexico
Received 14 March 2006; received in revised form 12 September 2006; accepted 13 September 2006
Available online 27 October 2006

Abstract

The galvanic effect between the main associated mineralogical phases in a mineral sphalerite concentrate was evaluated using
an alternative methodology. Comparative voltammetric studies were performed between high purity galena mineral (94.65%) and
sphalerite concentrate (content of 78.11% sphalerite, ZnS; 13.64% galena, PbS; 0.57% chalcopyrite, CuFeS2; 0.41% cadmium
sulfide, CdS; and 0.11% arsenopyrite, FeAsS) using carbon paste electrodes (CPE) in order to identify galvanic interactions that
affect their reactivity. The electrolyte was an aqueous solution of 0.1 M NaNO3 (pH 6.5). The results showed that, in sphalerite
concentrate, the electrochemical reactivity of the galena was diminished and displaced to more positive potentials with respect to
the high purity galena mineral response. This behavior can be attributed to the galvanic protection offered by the sphalerite on the
galena, thereby avoiding its free oxidation. On the other hand, sphalerite oxidation was diminished by the formation of a passive
products film that is dissolved to more positive potentials which provokes oxidation of other minerals like CuFeS2, (Zn,Cd)S and
FeAsS present in a minor proportion in the sphalerite concentrate.
2006 Elsevier B.V. All rights reserved.

Keywords: Galena; Sphalerite; Sulfide minerals; Galvanic interactions; Galvanic protection

1. Introduction pollution due to the emission of pollutant gases such as

In nature, sulfurous ores are generally complex mix-
tures, explaining why separation processes are not effi-
cient and the secondary products appear. Traditionally,
galena (PbS) and sphalerite (ZnS) minerals are the most
important raw materials to obtain base metals (Pb and
Zn, respectively) and generally are found associated
together. These sulfide minerals are treated with pyro-
metallurgical and hydrometallurgical techniques. The
first has been restricted because of the environmental
Corresponding author. Tel.: +52 771 71 72000x6713x6729; fax: +52
771 71 72000x6730.
E-mail address: reyescruz16@yahoo.com (V.E. Reyes).
0301-7516/$ - see front matter 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.minpro.2006.09.004
SO2. In the hydrometallurgical processes, the mineral or
metal dissolution is carried out with both oxidizing and
complexing agents that allow the metal sulfides of
interest to dissolve in solution. These processes are
known as oxidative dissolution because the reactions
involve charge transfer with the oxidation of the mineral
and the oxidizing agent undergoing its reduction. Today,
hydrometallurgical recovery is becoming a challenge
due to the secondary reactions provoked by the galvanic
interactions between minerals associated within the
concentrates, which affect the process. In the flotation
process, the galvanic interactions between two or more
minerals produce surface coatings that affect the float-
ability of sulfide minerals (Pozzo et al., 1990). It has
 G. Urbano et al. / Int. J. Miner. Process. 82 (2007) 148155
also been observed that the type of coating formed
depends, among other factors, on the mineral/solution
ratio (Ekmekci and Demirel, 1997). Meanwhile, in the
leaching process, the galvanic interactions could sub-
stantially increase the leaching of one or both of the
minerals, thus constituting a galvanic cell. Therefore,
galvanic cells originate when redox reactions occur on
sulfide minerals where the mineral with higher residual
potential acts as cathode and becomes galvanically pro-
tected. On the other hand, the mineral with the lowest
residual potential acts as anode and its dissolution be-
comes favored (Cruz-Gaona et al., 2003). Then, the
galvanic reactions will depend on the electrochemical
characteristics of minerals according to the occurrence of
different sulfides contained in the concentrates (Nowak
et al., 1984; Paramguru and Nayak, 1996; Abraitis et al.,
2003).
Generally, the galvanic interaction between sulfide
minerals has been studied using short-circuited galvanic
cells or with attached mineral electrodes and by com-
paring individual electrochemical behavior of the
minerals (Metha and Murr, 1983; Nowak et al., 1984;
Paramguru and Nayak, 1996; Madhuchhanda et al.,
2000). In these type of cells, the contact between mine-
rals is through an electrolytic solution while, in an
industrial concentrate, the electrical contact between the
mineralogical phases are in solid state. This difference
could explain the limited reliability of these galvanic
cells for the prediction of mineral reactivity.
Today, electrochemical techniques have become one
of the most powerful tools to study galvanic interactions
between different mineral associations under conditions
similar to those found in sulfide mineral concentrates. In
the use of these techniques, electrical conductivity is
very important. Most sulfide minerals have good con-
duction due to their semi-conductivity characteristics;
however, some do not have this property (i.e. sphaler-
ite). In this case, the use of carbon paste electrodes
(CPE) has allowed the application of electrochemical
techniques and, because of this, the knowledge of the
interactions of non-conducting sulfide minerals can be
reached (Ahlberg and sbjrnsson, 1993; Cisneros
et al., 1999). In the case of solid electrodes, there is a
percolation effect on the conductivity of the electrode
provoking a potential drop due to changes in current
resistance (IR) at the interface; however, on the CPE,
this effect is negligible, because of the hydrophobic
binding agent.
In this work, a comparative voltammetric study with
CPEgalena mineral was carried out in order to deter-
mine the effect of the galena on the sphalerite oxidation
and vice versa. An experimental strategy is presented in
149
order to understand the galvanic interactions of galena
and sphalerite contained in a mineral concentrate with the
presence of other sulfides. The electrochemical study
using CPEgalena mineral and CPEsphalerite concen-
trate (containing 13.64% of galena) was performed in
electrolyte containing 0.1 M NaNO3 at pH 6.5. This
electrolyte was used because it does not interfere with
electrochemical reaction of metallic sulfides and does not
form complexes with metallic cations (i.e. Zn, Cu, etc.);
thus offering an excellent medium for determining galva-
nic interactions affecting the reactivity of sulfide mineral
concentrates (Cruz et al., 2005).
2. Materials and methods
2.1. Minerals and reactants
A sample of galena mineral was collected from the
mine El Monte of the mining district of Zimapn
(Mxico) and a sample of sphalerite was collected as
concentrate from the beneficial plant of the same place.
These samples were ground in an agate mortar and
sieved to b74 m ( 200 mesh size).
Graphite used to prepare the working electrodes has
215 m particle size with 99.9995% of purity (Alfa-
Aesar). The silicon oil used as binding agent has a
0.963 g/ml(25 C) density and 200 cSt (25 C) viscosity.
Solution used was 0.1 M NaNO3 (pH 6.5, adjusting
with NaOH or HNO3). Deionized water with specific
resistance of 18.2 M cm 1 was used in preparing the
solution and all the reagents were analytic grade. Elec-
trolyte prepared this way was deaerated and preserved with
nitrogen atmosphere before and during all experiments.
2.2. Equipment and procedures
A typical three-electrode cell was conditioned with
nitrogen to maintain an inert atmosphere and to carry out
the electrochemical experiments at room temperature. A
graphite solid bar was used as the auxiliary electrode
and a standard sulfate electrode (SSE, E = 615 mV vs.
SHE), immersed in a Luggin capillary, as the reference
electrode. All potential values were converted to the
standard hydrogen electrode (SHE, by adding 0.615 V)
scale. Working electrodes were prepared by mixing
carefully the graphite powder and mineral with silicon
oil and later homogenizing in the agate mortar. The
ratios used for graphite powder and mineral were
20:80 wt.% in the case of galena and 60:40 wt.% in
the case of sphalerite. The latter was used due to low
reproducibility of the sphalerite electrochemical re-
sponse at lower ratios. Resulting pastes were located
150 G. Urbano et al. / Int. J. Miner. Process. 82 (2007) 148155

ical phases were observed with scanning electron micro-

scope (SEM; image shown in Fig. 1) and the chemical
analysis was carried out by inductively coupled plasma
(ICP). Mineralogical composition resultant is shown in
Table 1.

3.1. Electrochemical characterization of galena

Fig. 2 shows voltammetric responses of a CPEgalena

Fig. 1. SEM image of sphalerite concentrate containing the associated
mineralogical phases of sulfide minerals exemplified for sphalerite
(ZnS), galena (PbS), and arsenopyrite (FeAsS).
inside the CPE with a surface area of 0.0314 cm2 ex-
posed to the solution. Fresh surface was created for each
experiment by extruding the mineral paste and cutting
off the spent part. The electrochemical studies were
carried out using a PAR 263A Potentiostat with Power-
Suite Software of the same company.
3. Results
In order to analyze the galvanic interaction between
the galena and sphalerite, electrochemical behavior of
CPEgalena mineral was first determined and later the
CPEsphalerite concentrate oxidation was described.
The interaction between the minerals was explained by
comparison of both electrochemical responses.
The sphalerite and galena minerals were character-
ized mineralogically and chemically to determine the
stoichiometric composition of both minerals and the
contents of mineralogical impurities. Some mineralog-
electrode when positive and negative scans (ii and iii
respectively) were carried out, beginning at open circuit
potential (OCP) with a sweep rate () of 20 mV s 1. The
electrochemical behavior of the CPE (100% graphite) in
the positive direction was also shown in Fig. 2i for
comparative purposes. This last does not show oxidation
nor reduction representative responses in the whole of
potential range.
When the scan potential was initiated in positive
direction (Fig. 2ii), three oxidation processes were ob-
served: one small peak (A1) that begins near 0.6 V,
another peak (A2) reaches a maximum at 1.12 V, and
finally A3 increases as the potential scan becomes more
positive. When the scan potential was reversed, reduc-
tion process, C1, and oxidation peaks A4 and A5 were
observed. On the other hand, when the galena was
previously reduced (Fig. 2iii), a reduction process C1
and two oxidation peaks, A5 and A2, were observed.
This last process was wider and showed higher currents
than peak A2. Both processes were compared by means of
the charges associated and this comparison showed that in
peak A2 the transformation was higher (QA2 = 13.51 mC
and QA2 = 42.52 mC).
The analysis of the voltammograms obtained in both
scan directions showed that the galena oxidation was

Table 1
Mineralogical species percentage contained in galena mineral and
sphalerite concentrate
Sample Species (%)
Galena PbS 97.65
ZnS 00.67
CuFeS2 00.61
Sb2S3 00.25
Ag 1393 ppm
Sphalerite concentrate (Zn99.68,Cd0.32)S 85.13
PbS 13.64
Fig. 2. Typical cyclic voltammograms obtained on CPE-without
CuFeS2 00.57
mineral in positive direction (i) and CPEPbS 20:80 wt.% in 0.1 M
FeAsS 00.11
NaNO3 at pH 6.5 ( = 20 mV s 1) when the potential scan was initiated
Ag 73 ppm
in (ii) positive direction and (iii) negative direction.
 G. Urbano et al. / Int. J. Miner. Process. 82 (2007) 148155
associated to peaks A2 and A2, since both peaks have
similar behavior. While, the comparison between the
reduction processes C1 and C1 allows observing that
the current of process C1 increases when the mineral
was previously oxidized, indicating that the reduction
process C1 corresponds only to the reduction of the
galena mineral. Thus, it can be proposed that C1 corre-
sponds to the following electrochemical reaction:
PbS 2H2 O 2e Pb0 H2 S 20H ;
1
E 0:61V vs: SHE
The equilibrium potential, E, related to Eq. (1), was
calculated taking into account the corresponding stand-
ard potential, E for the reaction (Bard et al., 1985) and
considering a concentration of 10 6 M for the species
formed at the interface. This concentration is frequently
used in the case of metal corrosion or mineral con-
centrate leaching (Pourbaix, 1977).
Therefore, process C1 should be associated to the
reduction of the chemical species formed during the
oxidation processes (peaks A2 and A3) of galena and
the remaining galena.
In order to identify the different processes involved in
the galena oxidation, a voltammetric study was carried
out changing the positive switching potential, E+, be-
ginning the scan in the OCP at 20 mV s 1 (Figs. 3 and 4).
According to Fig. 3, peak A2 increases until a
maximum (at 1.12 V), then when the switching potential
(E+) was more positive than 1.2 V, the current asso-
ciated to the backward scan diminished. This behavior
has been generally associated to the formation of a
passive film on the electrode surface. Then, the oxidation
process associated to peak A2 of the galena response
Fig. 3. Typical cyclic voltammograms obtained on CPEPbS 20:80 wt.%
in 0.1 M NaNO3 at pH 6.5 ( = 20 mV s 1). The potential scan was
initiated in positive direction and the positive switching potential (E+)
was varied between 1.0E+ 1.4 V, with increments of 0.1 V. The
negative switching potential was fixed at 1.2 V.
151
Fig. 4. Typical cyclic voltammograms obtained on CPEPbS 20:80 wt.%
in 0.1 M NaNO3 at pH 6.5 ( = 20 mV s 1). The potential scan was
initiated in positive direction and the positive switching potential (E+)
was varied between 1.6E+ 1.8 V. The negative switching potential
was fixed at 1.2 V.
forms insoluble species of Pb(II). This behavior was
similar to that reported by Gardener and Woods (1979),
Lamache et al. (1981), Pritzker and Yoon (1987),
Chernyshova (2001), however the authors proposed
different insoluble species forming during the oxidation
of galena, as shown in Reactions (2a), (2b), (2c) and (2d).
PbSPb2 S0 2e ; E 0:194V vs:SHE 2a
PbS 4H2 OPbSO4s 8H 8e ;
2b
E 0:383V vs: SHE
PbS 2H2 OPbOH2s S0 2H 2e ;
2c
E 0:417V vs: SHE
PbS H2 OPbOs S0 2H 2e ;
2d
E 0:795V vs: SHE
An analysis of the more negative region of the back-
ward scans showed the formation of a reduction process,
C2, which increased as the inversion potential became
more positive (see inset of Fig. 3a). This process was
associated with the reduction of S0 and recombination of
formed sulfide and Pb2+ present in the interface leading
to the formation of PbS (Reaction (2a)).
In addition, metallic lead can deposit on the PbS
surface when the potential was more negative (Fig. 3,
peak C3; Costa et al., 2002; Gardener and Woods,
1979). At more negative potentials, a reduction process
C3 was observed to be wide and, like C2, to increase as
the E+ increases. It is worth mentioning that both
processes (C2 and C3) were not observed on the
152 G. Urbano et al. / Int. J. Miner. Process. 82 (2007) 148155

Table 2 cess A4 appeared (see inset of Fig. 4), while the re-
Determination of cathodic, anodic and ratio charges on CPEgalena, duction process C3 showed an increase in the current.
obtained from different positive switching potential voltammetries
The change in the form of the process C3 is related with
E+ (V vs. SHE) QA (mC) QC (mC) QA/QC the dissolution process of the galena mineral, which
(A1 + A2 + A3) (C2 + C3 + (C1))
becomes very important at potentials more positive than
1.0 7.92 11.44 0.69 1.5 V.
1.1 13.01 14.95 0.87
The integration of the cathodic and anodic charges (in
1.2 15.90 17.01 0.93
1.3 17.42 20.35 0.86 Table 2) of Fig. 3 yielded a charge ratio, QA/QC, less than
1.4 17.13 20.45 0.84 the unity between the potentials of 1.0 to 1.6 V, which
1.5 20.58 25.41 0.81 indicates that Reaction (1) takes place simultaneously
1.6 16.19 18.34 0.88 with any of Reactions (3a) (3b) (3c). On the other hand,
1.7 34.13 34.10 1.0
the charge ratio between potentials N 1.6 until 2.0 V
1.8 42.61 38.36 1.11
1.9 63.3 45.21 1.40 (Figs. 4 and 2ii) was higher than unity indicating that
2.0 59.22 37.02 1.60 some of Reactions (2a) (2b) (2c) (2d) are taking place
together with some of Reactions (4a) and (4b).

voltammogram of Fig. 2 (curve ii). Therefore, they are 3.2. Electrochemical characterization of the sphalerite
only associated to the reduction of the chemical species
formed in peak A2. Thus, peak C3 should correspond to The electrochemical behavior of the CPEsphalerite
the reduction of the different insoluble species of lead to was studied in a potential range similar to that used for
Pb0 according to the following reactions: galena. Typical voltammograms of the positive and
Pb2 2e Pb0 ; E 0:306V vs: SHE 3a negative scan on CPEsphalerite electrode were shown
in Fig. 5ii and iii, respectively. Both scans were initiated
PbOH2 2H 2e Pb0 2H2 O; from the OCP with a sweep rate () of 20 mV s 1.
3b
E 0:083V vs: SHE Response on CPE-without mineral is also shown (Fig. 5i)
for comparative purposes.
PbO 2H 2e Pb0 H2 O; When the potential scan began in negative direction
3c (Fig. 5iii), only a reduction process G5 was observed at
E 0:295V vs:SHE
more negative potentials and with lower current values
As anodic scan proceeded, the formation of a than peak G5 in Fig. 5ii. The reduction peaks G3, G4
characteristic fine oxidation peak (A5) was observed and G5 were only formed when the scan began on the
and could be attributed to the dissolution of metallic Pb positive direction, which indicates that these peaks are
according to Reaction (3a) (Pritzker and Yoon, 1988; associated to the reduction processes of products formed
Cisneros et al., 1999, 2000). during oxidation (processes E1 and E2).
Fig. 4 shows that, when E+ N 1.5 V, the voltammo-
grams presented a current increase (process A3) and an
activation process when the scan potential was reversed,
indicating that the passive film (probably PbSO4, as
mentioned above) formed in peak A2 was dissolved
(Gardener and Woods, 1979). At more positive
potentials, the oxy-sulfur species S2O32 and SO42 are
the most likely to be generated in peak A3 according to
the following reactions (Pritzker and Yoon, 1987):

2PbS 5H2 O2PbO S2 O2
3 10H 8e ;
4a
E 2:389V vs:SHE

PbS 5H2 OPbO SO2
4 10H 8e ;
4b
E 1:358V vs:SHE Fig. 5. Typical cyclic voltammograms obtained on CPE-without mineral
in positive direction (i) and CPEZnS concentrate 60:40 wt.% in 0.1 M
On the other hand, when the potential E+ became NaNO3 at pH 6.5 ( = 20 mV s 1) when the potential scan was initiated
more positive, the reduction peak C2 changed and pro- in (ii) positive direction and (iii) negative direction.
 G. Urbano et al. / Int. J. Miner. Process. 82 (2007) 148155 153

In order to corroborate that peak E1 corresponds to

the oxidation of sphalerite and to identify the response
attributed to the oxidation and reduction of the galena, a
particular study was performed on the CPEsphalerite
concentrate (Fig. 7). It was oxidized until a potential of
2.0 V and after the potential scan was reversed. Later,
cathodic scans were conducted to different negative
switching potentials and reversed back to the initial
potential on the OCP. This procedure allows detecting
the voltammetric response for all the oxidized species
produced until the potential of 2.0 V.
Fig. 7a shows the voltammograms with change in
lower potentials (E = 0.3 to 0.6 V). In the figure,
the evolution of the reduction peak G3 was observed
Fig. 6. Typical cyclic voltammograms obtained on CPEZnS and it could be associated with the oxidation products
concentrate 60:40 wt.% in 0.1 M NaNO3 at pH 6.5 ( = 20 mV s 1). formed during the anodic scan. It was related to the
The potential scan was initiated in positive direction and the positive
switching potential (E+) was varied between 0.8 E+ 1.2 V. The
oxidation peak E5 because it increased as the switching
negative switching potential was fixed at 1.2 V. potential became more negative. Processes G3 and E5
correspond to the Pb2+ reduction to metallic Pb and the
Taking into account that peaks E1 and E5 (Fig. 5ii) oxidation of metallic Pb to Pb2+, respectively, according
could be associated to the redox processes of galena to Fig. 3, peaks C3 and A5. This fact indicates that galena
(according to Pritzker and Yoon, 1987; Ahlberg and
sbjrnsson, 1994) and that the content of galena is
important in the sphalerite concentrate (see Table 1), a
study of inversion potential scan was carried out. This
study was only in the potential range of 1.2 and 1.2 V.
Fig. 6 shows different voltammograms obtained
with positive inversion potentials (E+ = 0.8 V to
1.2 V), keeping the negative inversion potential fixed
at 1.2 V. The potential scan was initiated on the
positive direction from OCP at 20 mV s 1. Fig. 6 shows
the evolution of the oxidation peak E1, which has been
associated to the reduction peak G5, since this latter
increase when the inversion potential becomes more
positive. The oxidation peak E5 also increased as
the inversion potential increased. A comparison of
Figs. 3 and 6 allows discarding the hypothesis that the
E1 process (in Fig. 6) corresponds only to the galena
oxidation, since the shape of the oxidation peak E1 and
reduction peak G5 was quite different to the
corresponding oxidation (A2) and reduction (C3)
peaks of galena (Fig. 3). On the other hand, presence
of the oxidation peak E5 of Fig. 6 indicates that only
a very small part of the galena was oxidized on the
direct scan (peak E1). Therefore, the simultaneous
presence of galena and sphalerite in the concentrate
provoked an important diminishing on the kinetics of
the galena dissolution. Thus, peak E1 corresponds to Fig. 7. Typical cyclic voltammograms obtained on CPEZnS
the sphalerite oxidation, producing insoluble sulfur spe- concentrate 60:40 wt.% in 0.1 M NaNO3 at pH 6.5 ( = 20 mV s 1).
The potential scan was initiated in positive direction and the negative
cies (probably S0) on the electrode surface. These in- switching potential (E) was varied between: (a) 0.3E 0.6 V,
soluble species could form a passive film that dissolves (b) 0.7 E 1.4 V. The positive switching potential was fixed
at more positive potentials. at 2.0 V.
154 G. Urbano et al. / Int. J. Miner. Process. 82 (2007) 148155
was oxidized at more positive potentials when sphalerite
was present.
On the other hand, if the switching potential became
more negative (Fig. 7b), the reduction peaks G4, G5 and
the oxidation peak E6 appeared. The reduction peak G4
was localized in the same potential range where a re-
duction process appeared on a previous voltammetric
study carried out on CPE-without mineral in a solution
with ionic cadmium (under the same conditions; see inset
of Fig. 7b). Peak G4 could be attributed to the reduction
of cadmium ions released during the oxidation of the
cadmium sphalerite, (Zn,Cd)S, present in the concentrate
(Table 1). On the other hand, peak G5 could be asso-
ciated to the reduction of Zn2+, which was produced
during the oxidation of the sphalerite concentrate in the
anodic direction of the scan. This fact was also verified
through a voltammetric study on CPE-without mineral in
solution with ionic zinc (like ionic cadmium, under the
same conditions), which was also shown in the inset of
Fig. 7b. When the voltammetric study was carried out
while stirring the solution (results to be submitted to
IJMP), a decrease on the current of peaks G3 and G5 was
observed, this behavior confirms the presence of ionic
species formed during the oxidation process.
4. Conclusions
Galena in sphalerite concentrate diminishes its
oxidation due to the presence of sulfide minerals with
Zn and Cd that causes a galvanic effect, which favors the
oxidation of the sphalerite and the other minerals before
galena oxidation. By comparison, galena in sphalerite
concentrate oxidizes at potentials more positive than
that obtained for high purity galena indicating that
mineral associations in the concentrate cause a decrease
in galena reactivity. This behavior is attributed to the
galvanic protection of the sphalerite on galena, thereby
avoiding its free oxidation. The presence of galena in the
concentrate allows observing sphalerite oxidation,
which generally is difficult to observe with pure spha-
lerite (Ahlberg and sbjrnsson, 1994). On the other
hand, the formation of a passive film, probably of ele-
mental sulfur, could prevent free sphalerite oxidation.
The formation of this passive film, that finally dissolves
at more positive potentials, provokes the oxidation of the
other minerals contained in the sphalerite concentrate as
the (Zn,Cd)S.
Acknowledgements
The authors would like to thank CONACYT and
Hidalgo's government for the financial support of the
Fomix Project 2002-01-9166. Gustavo Urbano Reyes
wishes to thank the doctorate scholarship provided by
CONACYT and the PIFOP program.
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