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Hydrometallurgy 89 (2007) 260 268

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Leaching of sulfide copper ore in a NaClH2SO4O2 media with

acid pre-treatment
O. Herreros a,, J. Vials b
a
b

Department of Mining Engineering, Universidad de Antofagasta, Casilla 170, Antofagasta, Chile

Department of Materials Science and Metallurgical Engineering, Universidad de Barcelona, Spain
Received 27 March 2007; received in revised form 3 July 2007
Available online 20 July 2007

Abstract
A study was made of the leaching of a sulfide copper ore in a NaClH2SO4O2 media after pre-treatment by agglomeration
with H2SO4(conc) and NaCl. The leaching variables evaluated included the amount of NaCl to be employed, the percentage of solids
in the leaching solution, particle size of the raw mineral to be leached, and the preferable method of agitation in the leaching
system. Mineralogical characterization of the material to be leached included analysis of the raw ore and of the leached ore residue
using reflected-light microscopy, X-ray diffraction, and scanning electron microscopy. The soluble species included djurleite and
digenite. The most important parameters in the leaching process proved to be particle size and type of agitation. A total percentage
of copper extraction of 70% was achieved using mechanical stirring, which increased to 78% when using compressed air agitation.
The best extraction of the copper was achieved when leaching with 3 g/L of chloride, room temperature of 20 C, and when all
particles were b 1.65 mm in diameter.
2007 Elsevier B.V. All rights reserved.
Keywords: Copper; Sulfides; Leaching; Chlorides

1. Introduction
The high degree of efficiency of the leaching power of
chlorides has been noted in numerous experimental studies
for the hydrometallurgical treatment of sulfide ores,
particularly the complex sulfides (Herreros et al., 2004;
Habashi, 1995; Peters, 1992; Winard, 1991). A number of
industrial processes have been designed based on these
studies, and differ mainly in terms of the oxidizing agents
employed, including Cu2+, Fe3+, O2, Cl2, and others. In all
cases, the leaching medium employed includes high
concentrations of chloride, obtained by adding sodium
chloride, or to a lesser extent calcium chloride or a mixture
Corresponding author.
E-mail address: oherrero@uantof.cl (O. Herreros).
0304-386X/$ - see front matter 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.hydromet.2007.07.011

of the two. In all these processes the saline additive

provides a sufficiently high concentration of chloride to
guarantee the leaching of the copper, lead, and silver from
the source mineral. The addition of calcium chloride allows
for the control of sulfates in solution (Vracar et al., 2000).
The majority of non-ferrous metals of interest are
water-soluble, promoted by the presence of chloride
ions. Generally, the leaching of the sulfides occurs more
easily in solutions of chloride rather than sulfate (Lu
et al., 2000a,b; Fisher, 1994; Fisher et al., 1992; Chu and
Lawson, 1991a,b). Maintenance of leaching power can
be achieved through oxidation, or by pyro-hydrolysis.
Solvent extraction is a powerful tool for purification of
the resultant leaching solutions.
The capacity of leaching processes employing chloride
to generate elemental sulfur without the alteration of

O. Herreros, J. Vials / Hydrometallurgy 89 (2007) 260268

pyrite makes them highly useful for treatment of complex

pyritic sulfides.
There is extensive information which suggests that
leaching with copper chloride at high temperatures and
Cl concentrations is controlled electrochemically (Parker et al., 1981a,b) and correlation also exists between the
mixed potential of the copper chloride medium and the
speed of the leaching (Majima et al., 1988). The higher
efficiency of CuCl2 solutions than those of FeCl3 is due
to the fact that the action of the Cu2+/Cu+ pair is quicker
and more reversible than that of the Fe3+/Fe2+pair on the
surface of chalcopyrite in the chloride medium. In a
strong chloride media, the predominant cuprous, cupric,
ferrous, and ferric species are, respectively, Cu2+,
CuCl32, CuCl+, CuCl2, FeCl2 and FeCl2+.
In a study on the leaching of djurleite in a Cu2+/Cl
media, Herreros et al. (2006) determined that the
leaching process followed:

Cu1:97 S 0:97Cu2
chlorocomplex CuS 1:94Cuchlorocomplex

1
when the conditions included Cu2+ 0.020.23M, Cl
0.61.3M and temperature 2080 C. These authors
determined that the kinetics of the process was
determined by the chemical reaction, with activation
energy of 35kJ/mol (8.4kcal/mol).
Some processes have been proposed in recent years for
leaching sulfides ores in chloride media, including the
Cuprochlor Process (Chilean Patent, 2001), and processes
for copper concentrates (CUPREX Process, Dalton et al.,
1991; CELS Process, Barr et al., 2000; INTEC Process,
Moyes and Houllis, 2002; HydroCopper Process, Hyvarinen et al., 2002). Also, Herreros et al. (2005) have
leached partially oxidized copper concentrates using
NaCl in an acid media, obtaining solutions containing
15 to 35 g L 1 copper and 2 to 5 g L 1 chloride, which
makes them useful for subsequent solvent extraction.
1.1. Theoretical framework
A study was made on the leaching of sulfide copper
ore using cupric-chloride complexes as a hydrometallurgical alternative to presently used methods. In this
alternative, the leaching agents Cu2+, CuCl+, CuCl2 and
CuCl3 are continuously generated during the leaching
process. This is produced from the soluble copper
contained within the mixture of sulfide ores under
treatment. Also, in the case of sulfide ores or concentrates, external copper sulfate may be added from
solutions available in the plant. The leaching is initiated
with the formation of copper complexes based on

261

thermodynamic data (Duby, 1977; HSC Outokumpu,

1999):
Cu2+ + Cl = CuCl+
CuCl+ + Cl = CuCl2
CuCl2(aq) + Cl = CuCl3
CuCl3 + Cl = CuCl2
4

(INCRA)
K1 = 100.45
K2 = 10 0.27
K3 = 10 2.48
K4 = 10 2.30

(HSC)
K1 = 100.474
K2 = 10 4.53
K3 = 101.767
K4 = 10 2.301

(2)
(3)
(4)
(5)

Which has shown in practice that, in the Cu2+/Cl

system, the main compounds are Cu2+ and CuCl+ based
on the distribution of species (Herreros et al., 2005).
The cupric ion and the cupric chloride complex
CuCl+ generated by reaction (2), would dissolve the
sulfide species following:
Cu2 S Cu2 2Cl CuS 2CuCl
G0 46:3 kJ=mol11:05 kcal=mol

Cu2 S CuCl Cl CuS 2CuCl

G0 43; 5 kJ=mol10; 4 kcal=mol

CuS Cu2 2Cl 2CuCl S

G0 25:8 kJ=mol6:2 kcal=mol

CuS CuCl Cl 2CuCl S

G0 23:0 kJ=mol5:5 kcal=mol

CuFeS2 3Cu2 6Cl

4CuCl FeCl2 2S0 G0
73:4 kJ=mol17:5 kcal=mol

10

CuFeS2 3CuCl 3Cl

4CuCl FeCl2 2S0 G0
65:3 kJ=mol15:6 kcal=mol

11

From this thermodynamic analysis, using values

obtained with the HSC software [Outokumpu, 1999], it
is observed that the Cu2+ has greater oxidizing power
than the CuCl+ and that the most favorable reactions are
those that generate solid CuCl before soluble CuCl2.
Due to the preceding, an important effect to be studied in
the leaching experiments is the concentration of chloride
most favorable to reactions which produce the formation
of CuCl2.
Reactions (6)(11) are thermodynamically the most
favorable under standard conditions. It is almost certain
that the main, if not the only product of the reactions is
CuCl.
The CuCl formed can be re-oxidized to give the
leaching copper complex, following:
2CuCl 1=2 O2 2H 2CuCl H2 O

12

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O. Herreros, J. Vials / Hydrometallurgy 89 (2007) 260268

continuing the dissolution reactions of the sulfide

species. Reaction (12) has a free energy value of
97.8kJ/mol ( 23.4kcal/mol).
Therefore, the leaching system requires the input of
oxygen, either as pure oxygen, or oxygen from the air, in
order to oxidize the cuprous products.
It is proposed that the leaching process of the sulfide
copper ore functions by means of copper-chloride
complexes and free oxygen following:
Copper sulfide 2Cu2 chloride complex
4Cu chloride complex S

13

2Cu chloride complex 2H 1=2 O2

2Cu2 chloride complex H2 O

14

This analysis only presents a hypothesis for the

phenomenology of the process, and is presently based
on limited experiments and measurements. More
detailed research may be needed in the future to confirm
that this process occurs in the form hypothesized.
The main objective of the present research was to
investigate the use of a copper chloride complex (CuCl+)
for the leaching of Cu2xS-type phases (djurleite, digenite)
present as the main constituents of the tested sulfide
copper ores, using an oxidizing mixture composed of
sulfuric acid, sodium chloride, and an input of soluble
copper from the ore in various experimental proportions.
Evaluation of the effects of different total chloride
concentrations is proposed, as well as particle size of the
ore in treatment, and the type of stirring (mechanical or
compressed air).

Table 1
Percentage of species presents in the sulfide copper ore
Species

Percentage

Cu2 xS phases (djurleite, digenite)

Chalcopyrite
Covellite
Enargite
Bornite
Pyrite
Gangue

1.45
0.39
0.11
0.09
0.14
1.67
96.15

2.1.2. Analysis by X-ray diffraction

Analysis by X-ray diffraction showed the presence of the
following mineralogical species in the original ore sample:
Original ore:
Major: Quartz (SiO2) N Muscovite [Kal2(Si3Al)O10
(OH,F)2] N Djurleite (Cu31S16) N Digenite (Cu9S5)
Minor: Pyrite (FeS2) N Pyrophyllite [Al2Si4O10(OH)2] N
Illite [(K,H3O)Al2Si3AlO10(OH)2] N Chlorite [(Mg,Fe)6
(Si,Al)4O10(OH)8] N Kaolinite [Al2Si2O5(OH)4] N Chalcopyrite (CuFeS 2 ) N Molybdenite (MoS 2 ) N Hematite
(Fe2O3).
Selected samples from the leaching process were
analyzed using XRD and SEM-EDS (Section 3.6, below).
2.2. Reagents
In all the leaching experiments we employed
technical grade concentrated sulfuric acid and analytical
grade sodium chloride.
Chemical analysis of copper in leached solutions was
carried out using atomic absorption spectrometry (AA)
and free acidity was determined using the sodium
carbonate method.

2. Materials and reagents

2.3. Experimental procedure
2.1. Materials
The raw material treated in this study was sulfide
copper ore supplied by a mining industry in the
Antofagasta (Chile) region. The particle size of the
mineral samples used in the study was less than
1.65 mm in major diameter, except in the experiments
on the effect of particle size in the leaching process. The
composition of the mineral was 0.22% soluble copper
and 2.01% total copper. The consumption of acid in the
determination of soluble copper was 0.022 g acid/g
mineral.
2.1.1. Mineralogical analysis
The mineralogical analysis was made using reflectedlight microscopy, with results given in Table 1.

2.3.1. Mineral pre-treatment

The pre-treatment consisted of adding concentrated
sulfuric acid to a determined mass of ore based on the
consumption of acid and sodium chloride related to the
concentration of chloride desired in solution. This
mixture (agglomerate) was allowed to stand for 8days
at room temperature ( 20 C). For the leaching process,
water was added as needed.
2.3.2. Kinetic experiments
Some leaching experiments were carried out using a
one-liter capacity cylindrical reactor.
The pulp was prepared by adding a certain quantity of
pre-treated ore to a solution containing a pre-established
quantity of sulfuric acid. This pulp was stirred using a 5-cm

O. Herreros, J. Vials / Hydrometallurgy 89 (2007) 260268

263

Fig. 1. Percentage extraction of total Cu vs time, as a function of NaCl

concentration. (20 C, 400 rpm, 8 g L 1 H2SO4, d0 = 1.65 mm,
pH = 1.561.67, 295305 mV).

Fig. 3. Percentage extraction of total Cu vs time, as a function of the

percentage solids present (20 C, 400 rpm, 8 g L 1 H2SO4,
d0 = 1.65 mm, pH = 1.561.67, 295305 mV).

diameter teflon stirring propeller, with a speed of 400 rpm

in all the leaching tests employing mechanical agitation.
A two-liter cylindrical reactor measuring 58 cm in
height by 7.8 cm in diameter was used for leaching tests
employing compressed air agitation. One liter volumes of
pulp, as described in the preceding (mechanical agitation)
were used in these tests. Compressed air was fed into the
mixture at 0.3 L/min. using a laboratory air pump.
The variables measured in these tests included the
percentage of solids, addition of sodium chloride,
particle size, and type of agitation.

These tests, considered as preliminary, were carried

out with 1000 ml of solution containing about 10%

solids by weight (111 g of mineral), mechanical

agitation at 400 rpm, mean particle diameter of
1.65 mm, and sulfuric acid concentration of 8 g L 1.
The chloride concentrations varied from 0 to 10 g L 1.
The results for total copper extraction obtained in
these leaching tests are shown in Fig. 1.
From the results obtained it can be concluded that the
chloride concentration had only a minor effect in the
leaching tests in the range tested, showing that 54.4% of
the total copper extraction occurred when using the
equivalent of 3 g Cl, in comparison with an increase to
only 56.5% when using the 10 g Cl level. Thus all
subsequent leaching tests were done using 3 g Cl/L.
The remaining acid content in these tests was about
3 g/L which was low enough to make the solutions
amenable to subsequent solvent extraction (SX). The
dissolution of Fe was minor that 10ppm. Arsenic was
not detected in the leaching solutions.

Fig. 2. Percentage extraction of total Cu vs time as a function of

chloride concentration with compressed air stirring. (20 C, 0.3 L/min,
8 g L 1 H2SO4, d0 = 1.65 mm, pH = 1.561.67, 295305 mV).

Fig. 4. Percentage extraction of total copper vs time as a function of

particle size. (20 C, 400 rpm, 10% de slidos, 3 g Cl/L, 8 g L 1
H2SO4, pH = 1.561.67, 295305 mV).

3. Results and discussion

3.1. Effect of sodium chloride

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O. Herreros, J. Vials / Hydrometallurgy 89 (2007) 260268

The results obtained in these leaching tests are given

in Fig. 2.
These results showed that the leaching with stirring
by compressed air increased the percentage extraction of
total copper over that with mechanical stirring. As in the
preceding case, the leaching tests differed little in regard
to the presence of NaCl and thus the leaching tests were
continued using 3 g Cl/L.
Since the length of time of the leaching process did not
greatly affect the amount of copper extracted, after the first
hour, further testing was limited to one-hour durations.
Fig. 5. Percentage of total copper extraction vs time as a function of the
type of stirring applied to the leaching process (white points represent
air stirring, and black points mechanical stirring, T = 20 C, pH = 1.56
1.67, 295305 mV).

3.2. Effect of chloride concentration with compressed

air agitation
In this case the application of compressed air was made
to the leaching system. Here the amounts of chloride
ranged between zero and 10 g Cl/L, under the same
conditions as the first chloride test. The leaching was done
in the cylindrical reactor, applying 0.3 L air/min.

3.3. The effect of varying the percentage of solids in the

leaching test, maintaining a constant proportion of
chloride
These tests were carried out 1000 mL volumes of
solution, varying their percentage solids, and using a
constant relation between the g Cl/% solids, equivalent
to 3 g Cl /10% solids, as used in the preceding tests. The
leaching lasted 60 min at solids contents of 20%, 25%
and 30% , at 20 C, with 8 g L 1 H2SO4 and mechanical
stirring at 400 rpm.
The results of these leaching tests are shown in
Fig. 3.

Fig. 6. X-ray diffraction spectra of the sulfide mineral and the leached residue.

O. Herreros, J. Vials / Hydrometallurgy 89 (2007) 260268

Fig. 7. Amplified spectrum of the sulfide mineral and the leached residue showing the disappearance of the djurleite peaks.

Fig. 8. Amplified spectrum of the sulfide mineral and the residue, showing appearance of the 100 peak of the CuCl.

265

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O. Herreros, J. Vials / Hydrometallurgy 89 (2007) 260268

3.5. Comparisons between mechanical and compressedair stirring

Fig. 9. General appearance of the original ore. (SEM/BSE, 1: Cu2 xS,

2: pyrite, 4: quartz, 5: muscovite).

These tests showed that variation of the percentage

solids within the range tested had essentially no effect
among these leaching tests when the amount of chloride
is maintained in the same ratio to the amounts of solids
in all the tests.
3.4. Effect of particle size
The tests were carried out using 1000 ml of solution,
with 10% solids by weight, mechanical stirring at
400 rpm, 3 g Cl/L, 8 g L 1 H2SO4 . Leaching tests
were carried out separately on mean particle sizes of
0.98, 0.25 and 0.12 mm.
The results obtained from the leaching tests are
shown in Fig. 4.
It was evident from the preceding data that the
smaller the particle size, the greater the percentage of
extraction of the total copper.

Fig. 10. General appearance of the leached residue (SEM/BSE, 2

Pyrite, 4 Quartz, 5 Muscovite).

These tests were carried out with 1000 mL of

solution containing different amounts of solids, and
using a constant ratio of Cl, per g of solids as described
above. Air-stirred tests received 0.3 L of air per minute
and mechanically stirred tests at 400 rpm, for 60 minute
periods. Leaching tests were carried out with 10%, 20%,
25% and 30% solids in the solutions.
The results of these leaching tests are shown in
Fig. 5.
The results showed that air-driven stirring favored
the extraction of the copper in the leaching process. The
preceding is explainable in terms of oxygen consumption by the CuCl(solid) formed during the leaching
process, following:
2 CuCl 1=2 O2 2H 2CuCl H2 O

15

3.6. Characterization of the leached residue

To determine the sulfides species which were
attacked in conditions of 20 C, 3 g/L Cl , 8 g/L H+,
0.3 L/min air, and particle size b 1.65 mm, a sample of
the residue was analyzed by XRD and SEM-EDS.
The general spectra of the sulfide mineral and the
residue derived from it by leaching are compared in Fig. 6.
The main components of both samples were quartz and
muscovite ,with pyrophyllite and pyrite as minor components. Fig. 7 shows an amplified region of the spectrum in
which the presence of djurleite is seen as a minor phase in
relation to the overall composition. No other phases of
copper were detected using this method, which indicated
that the djurleite was the main phase containing this

Fig. 11. Original ore. Detail of the pyrite (2) partially replaced by
djurleite (1) (SEM/BSE).

O. Herreros, J. Vials / Hydrometallurgy 89 (2007) 260268

267

Based on the preceding analysis, and given that the

mineral contained very little soluble copper, this does
not appear to be the leaching agent, at least in the initial
phase of the leaching. As a mechanism, we propose:
Cu2 S 1=2 O2 2 H 4 Cl 2 CuCl2 S H2 O

16
Also, the CuCl2 generated could also be oxidized by
oxygen in the air:
2 CuCl2 1=2 O2 2H 2 CuCl 2 Cl H2 O
17
Fig. 12. Leached residue. Pyrite (2) showing the complete leaching of
the intergranular djurleite with which it was originally associated.
Traces of unattacked chalcopyrite (3) can be noted. (SEM/BSE).

and the CuCl+ generated in (17) could participate in

parallel to (19) in the leaching of the sulfide:
Cu2 S 2 CuCl 2 Cl 4 CuCl S

element. Fig. 7 also presents the spectrum of the residue

from which the djurleite phase has disappeared.
Fig. 8 shows another amplified region of the
spectrum. A minor 100 peak of CuCl residue was
detected, which indicated generation of this product
during the leaching process.
The general aspect of the mineral as determined by
electron microscopy is shown in Fig. 9. Its coarse
particle size is notable, and that the particle size range is
between 0.5 and 1.0 mm. Most of the particles are quartz
and muscovite. Minor amounts of sulfides are noted,
representing pyrite, and many of these are associated
with djurleite. The general aspect of the residue is
presented in Fig. 10. There is some increase in small
particles, perhaps due to abrasion phenomena. Unaltered
pyrite is detected, and djurleite is absent.
Fig. 11 shows the detail of a pyrite grain partially
replaced by djurleite (Cu2 xS). This phase is that which
contains most of the copper in this ore. Other sulfides
such as covellite and chalcopyrite occur in trace
amounts. Note that the replacement begins over the
surfaces of the pyrite grains, and also progresses through
the fissures, forming veinlets of copper sulfide. This
appears favorable for the potential leaching of the
copper sulfides since once it is initiated, it can proceed
along the veinlet. Thus special milling is not required for
the hydrometallurgical liberation of the copper.
Fig. 12 shows an analogous detail of the leached
residue. It can be noted that both the surface of the
djurleite as well as its fissures have been completely
leached, with representative empty spaces appearing in
the image. Note that the traces of chalcopyrite have not
been leached under these conditions. Also, no solid
CuCl was detected in the interstices of the pyrite.

18

and the CuCl formed could also be oxidized by oxygen

in the air, following:
2 CuCl 1=2 O2 2 H 2 CuCl H2 O

19

4. Conclusions
1.- The leaching of sulfide copper ores of the djurleite
and digenite type was effective through agglomerative pre-treatment with H2SO4(conc) and NaCl,
followed by leaching in an NaClH2SO4O2
media at room temperature.
2.- The leaching process was only weakly affected by
the quantity of sodium chloride added. For a
mineral containing 2.01% total copper in the forms
of djurleite and digenite, addition of the equivalent
of 3 gpl Cl was sufficient for the process.
3.- The percentage extraction of total copper was
notably favored when using agitation by compressed air, due to the input of free oxygen.
4.- With the presently tested mineral, the addition of
3 g de chloride/111 g of mineral was effective,
obtaining total copper extractions of above 70%.
5.- The particle size had a significant effect on the
leaching process, reaching percentages of above
90% when working with mineral whose particle
size was less than 1.65 mm in major diameter.
Acknowledgements
The authors thank the Office of Research of the
Universidad de Antofagasta and the Center for Mining
Scientific Research and Technology (CICITEM) for
partial financing of this study. We also thank the Serveis

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O. Herreros, J. Vials / Hydrometallurgy 89 (2007) 260268

Cientifics-Tcnics of the Universidad de Barcelona for

their help in descriptions of the minerals in this study.
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