Journal of Colloid and Interface Science 282 (2005) 408–414

www.elsevier.com/locate/jcis

Fundamental considerations on the mechanisms of silver cementation

onto zinc particles in the Merril–Crowe process
G. Viramontes Gamboa a , M. Medina Noyola a , A. López Valdivieso b,∗
a Instituto de Física, Universidad Autónoma de San Luis Potosí, Av. Manuel Nava No. 6, San Luis Potosí, S.L.P., C.P. 78210, Mexico
b Instituto de Metalurgia, Universidad Autónoma de San Luis Potosí, Av. Sierra Leona No. 550, San Luis Potosí, S.L.P., C.P. 78210, Mexico

Received 8 June 2004; accepted 17 August 2004

Available online 11 November 2004

Abstract
Studies on the Merrill–Crowe process as applied to silver recovery have shown that one half of the used zinc powder is wasted in water
reduction at high cyanide concentrations, while the other half reduces silver ions from the cyanide solution. However, the cementation
mechanisms as an electrochemical process taking place on the zinc surface do not explain the split of the electric current resulting from
the anodic dissolution of zinc into two equal values. This study demonstrates that the mechanism for silver precipitation at high and low
cyanide concentrations differs considerably. At low cyanide concentrations cementation is essentially an electrochemically-controlled process
following a shrinking-core behavior. At high cyanide concentrations, the process seems not to be electrochemically controlled. The areas for
zinc dissolution and silver deposition are not connected by an electrical-conducting medium and reduction of silver–cyano complex ions
takes place by hydrogen adsorbed onto silver growing outward from the cementing zinc particles. The results are based on scanning electron
microscopy of solids recovered from cementations in stirred reactors and in situ observations by optical microscopy of the cementation
process on the edge of thin zinc disks in cyanide solutions.
 2004 Elsevier Inc. All rights reserved.

Keywords: Silver; Metal cementation; Cyanide leaching; Zinc; Mineral processing

1. Introduction theoretically has a maximum value ε = 2, since one mole

The Merril–Crowe process for recovering gold and silver
from cyanide-leached ores has been widely used throughout
the entire world since its introduction at the end of 19th cen-
tury. The acquisition of zinc powder represents one of the
main investments for the plants that use this process, a suit-
able optimization of its consumption being clearly desirable.
Undesirable waste of zinc has its origin mainly in three
causes: (a) unconsumed zinc left in the precipitate, (b) im-
purities precipitation, and (c) other zinc-consuming side re-
actions. Together, these effects diminish zinc efficiency to
recover silver drastically. The cementation efficiency ε, de-
fined as the molar ratio of cemented silver to dissolved zinc,
* Corresponding author.
E-mail address: alopez@uaslp.mx (A. López Valdivieso).
0021-9797/$ – see front matter  2004 Elsevier Inc. All rights reserved.
doi:10.1016/j.jcis.2004.08.151
of zinc reduces two of Ag(CN)− 2 . However, in silver recov-
ery plants ε has a value around or lower than 1 [7,10,11].
In laboratory experiments the effects of impurities may be
controlled, and it has been shown that ε = 1 for high free
cyanide concentrations, like those commonly used in plant
practice [1,12]. This means that water reduction accounts for
one half of the used zinc, which is true under various exper-
imental conditions, like different silver and cyanide concen-
trations and lead ions in solution. Understanding the origin
of the ε = 1 relation has fundamental importance and con-
stitutes the aim of this paper.
It is generally accepted that the main chemical reactions
involved in the cementation of silver from cyanide solu-
tions using metallic zinc powder are of an electrochemical
nature. This means that the respective half reactions are
connected by an electrically-conducting medium, through
which an electric current is established transporting elec-
 G. Viramontes Gamboa et al. / Journal of Colloid and Interface Science 282 (2005) 408–414
Fig. 1. Schematic representation of the electrochemical behavior of silver
cementation onto zinc in the Merril–Crowe process.
trons from the zinc oxidation sites up to the silver reduc-
tion sites. A schematic picture of this process, as shown in
Fig. 1, is included in most scientific reports dealing with the
Merril–Crowe method to illustrate the cementation process.
Accordingly, electrochemical techniques have been exten-
sively used to delineate the mechanisms of precious metal
cementation in order to optimize plant operations [2–6,8].
In the Merril–Crowe process as applied to silver recovery
from cyanide solutions, the zinc oxidation and silver reduc-
tion reactions are
Zn0 + 4CN− → Zn(CN)2− −
4 + 2e ,
Ag(CN)− − −
2 + e → Ag + 2CN ,
0 (2)
respectively. If side reactions are absent the final stoichiom-
etry is
Zn0 + 2Ag(CN)− 0 2−
2 → 2Ag + Zn(CN)4 .
The cementation efficiency for Reaction (3) is ε = 2, the the-
oretical maximum. This value has been found to be true only
at low free cyanide concentrations, however [1]. As pointed
out above, ε is always closer to 1 than 2 in plant operation.
Besides impurities cementation, the decrease in ε has been
assigned to the simultaneous and wasteful consumption of
electrons by the following side reactions [9]:
O2 + 2H2 O + 4e− → 4OH− ,
1
H2 O + e− → OH− + H2 ,
2 alkaline silver–cyanide solution at initial pH 10.8. The so-
Reaction (4) is minimized in Merril–Crowe plants by
deaeration of the pregnant solution prior to the zinc powder
addition. Reaction (5) is less manageable since it depends on
the free cyanide concentration, which is determined by the
leaching conditions. Water reduction was recognized as the
most electron consuming side reaction soon after the imple-
mentation of the Merril–Crowe method [10,11]. Ever since it
has been the main explanation for the loss in zinc cementa-
tion efficiency. In adequately deaerated pregnant solutions,
Eqs. (2) and (5) are the main reduction reactions. Thus, if
409
the rates for both reactions are the same, instead of (3), the
overall silver cementation reaction should be
Zn0 + Ag(CN)−
2 + H2 O + 2CN
−
− 1
→ Ag0 + Zn(CN)2−
4 + OH + H2 . (6)
2
For this reaction ε = 1, since one mole of zinc precipi-
tates one of silver. This ε value and Reaction (6) have been
verified not only in controlled laboratory experiments at
high cyanide concentrations [1,12], but also in plant oper-
ations [7,9,11].
According to the traditional view of silver cementation
as an electrochemical process, the decrease in ε from its
maximum value of 2 to 1 seems to be a subject easy to be
understood. It would appear that the cause is a gradual in-
crease in water reduction as cyanide concentration increases,
taking place simultaneously in the electrochemical process.
Despite this apparent simplicity the issue is much more com-
plex, since it is necessary to point out that silver and water
reduction rates should be of the same order for Reaction (6)
to be valid. Taking into account that this is true for conditions
as varied as those in plant operations, there is no reason for
both rates to have similar values. In fact, both rates may be
completely different, as shown by the studies on the cemen-
tation of precious metals from cyanide solutions using Evans
diagrams by Parga [6]. This researcher did not detect hydro-
gen evolution in the cementation of silver, which occurred
(1)
in gold cementation as reported elsewhere [2,3,5,6]. It can
be stated that equality between both rates is not the rule,
but the exception, as deduced from electrochemical stud-
ies [2,3,5,6]. A congruent explanation of the origin of ε = 1
is really absent in the literature.
This work aims at thoroughly understanding the mecha-
(3) nism of the transition between Reactions (3) and (6) through
two different kinds of experiments. The first one was devised
to model the Merril–Crowe process through cementation
tests in stirred reactors. The second was aimed at explicitly
analyzing the validity of an electrochemical behavior for sil-
ver precipitation onto zinc at high cyanide concentrations.
2. Experimental
(4)
For all experiments, deionized water and analytical grade
(5) AgNO3 , NaCN, and NaOH reagents were used to prepare
lutions were purged with oxygen-free highly pure N2 to
remove O2 prior to the zinc addition and along all the ce-
mentation period.
In the first set of experiments, zinc powder cementation
tests were carried out in a 2.5 L glass reaction vessel im-
mersed in a temperature-controlled water bath. The zinc was
added when the O2 concentration was lower than 0.2 mg/L.
After 1 h the cementation products were collected through
filtration with 0.22-µm pore size filters and observed and an-
alyzed using a Phillips XL 30 scanning electron microscope
410 G. Viramontes Gamboa et al. / Journal of Colloid and Interface Science 282 (2005) 408–414
Fig. 2. (a) Schematic view of the zinc disk. (b) Two-dimension-like system
with epoxy resin to avoid the precipitation of silver on the zinc disk faces.
with accessories for chemical analysis. The solutions were
assayed for zinc and silver by atomic absorption spectropho-
tometry.
The second set of experiments consisted of the cemen-
tations of silver in a two-dimension-like system. They were
devised to elucidate if the areas of zinc dissolution and sil-
ver precipitation are or are not continuously connected by an
electrically-conducting medium. Fig. 2 shows schematically
a thin disk of metallic zinc whose faces were covered with an
insulating transparent epoxy resin. Only the zinc disk edge
was exposed to the silver–cyanide solution. Solutions were
prepared with initial AgNO3 and NaCN concentrations of
3.7 mM and 0.111 M, respectively. After O2 removal the
silver–cyanide solution was continuously pumped, through
a hose system, to fill a sealed Petri box containing the
zinc disk. The cementation evolution was directly observed
with a transmission optical microscope and recorded with
a coupled video-microscopy system. For silver and cyanide
concentrations used in these experiments, the cemented sil-
ver grows radially away from the disk edge while the zinc
disk shrinks. The formation of hollow spaces separating sil-
ver and zinc was manifested as bright areas in this two-
dimension-like system. The formation and subsequent evo-
lution of a continuous bright hoop demonstrates that silver
can be cemented in the absence of physical contact with
metallic zinc. A BUEHLER EPO-THIN low viscosity epoxy
resin No. 20-8140-032 and hardener No. 20-8142-016 were
used at a weight proportion of 100 parts resin to 36 parts
hardener, cured under room conditions. The electrical resis-
tivity of the cured product is ρ = 1.0–1.2 × 1016  cm−1 .
3. Results and discussions
Fig. 3 shows the ε dependence on the cyanide concentra-
tion, which is indicated as [NaCN]0 /[Ag]0 ; where [NaCN]0
and [Ag]0 are the total initial cyanide and silver concentra-
tions in mol/L, respectively. The tests were carried out with
[Ag]0 = 0.927 mM and [NaCN]0 was varied. The curve ex-
hibits three cyanide concentration regimes: the low cyanide
concentration regime given by [NaCN]0 /[Ag]0 ratios slightly
larger than 2, where the concentration of free cyanide ions
in solution starts to be significant and ε ≈ 2; the high
cyanide concentration regime occurring at [NaCN]0 /[Ag]0
ratios larger than 8, where ε ≈ 1; and finally, the interme-
Fig. 3. Silver cementation efficiency ε as a function of cyanide concentra-
tion.
diate cyanide concentration regime at [NaCN]0 /[Ag]0 ratios
between the two previous values, where ε decreases gradu-
ally from 2 to 1. The ε behavior in the figure does not depend
on the zinc particle size and remains unaltered if lead ions
are present in the solution. According to this result, around
one half of the electrons supplied by Reaction (1) is wasted
in water reduction in the high cyanide regime. The other half
reduces silver according to Reaction (2).
Fig. 4 shows the cementation patterns at different cyanide
concentrations. In the low cyanide regime the silver cemen-
tation follows a shrinking core behavior around the zinc
particles (Fig. 4a). In contrast, in the high cyanide regime,
where ε ≈ 1, the cemented silver always grows outward, into
the aqueous solution (Fig. 4b). In addition, if free cyanide
concentration is sufficiently high, cemented silver develops
branched morphologies independently of zinc size (Fig. 4c).
In the high cyanide regimen zinc particles progressively re-
duce their size inside a hollow space, which has exactly the
same shape as that of the original zinc particle. In the cyanide
regime where ε changes from 2 to 1 mixed behavior may be
detected.
To demonstrate that silver outward growth began instan-
taneously upon zinc addition at high cyanide conditions,
cementation tests with zinc particles having a rough tex-
ture on its surface were carried out (Fig. 5a). Fig. 5b shows
the characteristic texture of the inner face of the silver shell
cemented with this zinc. Comparison of both images demon-
strates that the initial texture and shape of the zinc particles
is printed on the inner side of the silver shells. All analyzed
particles follow this pattern. Because the shape of the in-
ner cemented silver–solution interface remains intact up to
the end of the cementation test, it can be stated that silver
cementation takes place only on the outer cemented silver–
solution interface.
The cementation of silver in the high cyanide regime can
then be pictured as a silver shell growing around a hollow
space and having an inner shape and size of the original zinc
particle. Inside this hollow space the zinc particle progres-
sively reduces its size. Additionally, the hollow space is free
of Ag(CN)− 2 complexes. Otherwise they would be cemented
either on the zinc particle or on the inner face of the silver
 G. Viramontes Gamboa et al. / Journal of Colloid and Interface Science 282 (2005) 408–414
Fig. 4. Silver cementation patterns. (a) Shrinking-core behavior in the low
cyanide concentration regime. (b) Outward growth at high cyanide concen-
tration regime. (c) Outward growth with development of dense-branched
silver morphology, also in the high cyanide regime.
shell; these possibilities, however, have not been confirmed
experimentally.
The transition of ε from its maximum value of 2 to 1,
takes place together with a transition in the cementation
pattern, from a shrinking core behavior to an outward sil-
ver growth. This suggests the possibility that the final value
ε = 1 at high cyanide concentrations is a consequence of a
morphological and stoichiometric transition. From Figs. 4b,
4c, and 5, it seems that the zinc particle separates from the
silver shell right at the beginning of the cementation reac-
tion. These observations lead to the hypothesis that in the
411
Fig. 5. (a) Characteristic texture of initial zinc particles. (b) Texture of the
inner face of the cemented silver shell at the high cyanide concentration
regime.
high cyanide regimen, where ε = 1, between the zinc parti-
cle and the silver shell there is no physical contact. If this
hypothesis is true, as experimentally shown below, the elec-
trons needed to reduce silver on the outer face of the silver
shell do not come directly from the zinc oxidation areas
located on the zinc surface. Instead, a chemical species is
produced directly on the zinc surface, diffuses through the
solution inside the hollow space and the pores of the silver
shell, and finally reduces silver–cyano complex species at
the cemented silver–aqueous solution interface.
Direct measurements of the interaction energy between a
metallic sphere (zinc) inside another hollow particle (silver
shell) filled with a multiple electrolyte (cyanide solutions)
are really difficult. Confronted with the difficulty of obtain-
ing directly this data, the zinc disk experiments were de-
signed to explicitly avoid the physical contact between zinc
and its respective silver shell. The idea was to demonstrate
the truthfulness of the hypothesis by deliberately avoiding
that physical contact between cemented silver and the ce-
menting zinc particle. If silver cementation stops then the
physical contact is a necessary condition. Oppositely, if it
continues then the cementation process should take place
following a mechanism distinct from that conventionally ac-
cepted.
412 G. Viramontes Gamboa et al. / Journal of Colloid and Interface Science 282 (2005) 408–414
Fig. 6. (a) Bright hoop separating the zinc disk and the cemented silver.
(b) Gas bubble detected inside the hollow space. (c) Growth of silver out-
ward from the bright hoop.
Silver cementation carried out in two-dimensional sys-
tems like the zinc disk additionally allowed a direct obser-
vation of the evolution of the hollow space separating ce-
mented silver and metallic zinc. Fig. 6 shows the result of
a cementation experiment on the zinc disk after 48 h. The
continuous bright hoop in this 2D system corresponds to
the hollow space in the zinc powder cementations. It is sur-
rounded by silver on the outer side and zinc on the inner side.
As the cemented silver grows outward the zinc disk shrinks;
the bright hoop expands separating completely both metals
(Figs. 6a and 6c). Additionally, Fig. 6b shows gas bubbles
detected inside the hollow hoop, with high probability they
are H2 bubbles. Because the epoxy resin is an excellent insu-
lator, this experiment demonstrates that the electrochemical
mechanism depicted in Fig. 1 is far from reality in the high
cyanide regime, where ε = 1. The electrochemical view is
only supported for low and intermediate cyanide regimes as
Fig. 4a clearly shows.
Zinc disk experiments demonstrate that silver cementa-
tion in the high cyanide regimen does not necessarily need
the electrical continuity between the areas for zinc dissolu-
tion and silver deposition. The results can only be explained
on the basis of two chemical reactions taking place at dif-
ferent interfaces and coupled only by a transport process
through the hollow space. Even though the chemical identity
of the species that reduces silver on the outer silver–solution
interface has not been determined exactly in this study, there
are reasons to believe that hydrogen is the most likely can-
didate. Hydrogen is produced at the zinc–aqueous solution
interface at such an extent that hydrogen bubbles are directly
observed inside the hollow space of the zinc disk experi-
ments. Thermodynamically, silver reduction with hydrogen
from cyanide solution is not excluded. Gas desorption tests
by pyrolysis, as detected by mass spectrometry, carried out
at high vacuum on the solids recovered from the zinc pow-
der cementations, indicate the codeposition of H, H2 , and
HCN. This possibility should be taken carefully since homo-
geneous reduction of silver from alkaline cyanide solutions
with pressurized H2 has been reported to be unlikely due to
high stability of the hydrogen molecule [13,14]. However, it
is well known that Cu2+ , Ag+ , and Hg2+ can activate mole-
cular hydrogen to make it more reactive as has been pointed
out by Osseo-Asare [15]. Thus, the formation of less alka-
line microenvironments around the cemented silver–cyanide
solution interface may lead to the activation of molecular
hydrogen through the stabilization of low concentrations of
Ag+ . As noted above, the absence of Ag(CN)− 2 molecules
inside the hollow space demonstrates the formation of mi-
croenvironments having properties different from those in
the bulk cyanide solution.
The electrochemical mechanism as shown by Eqs. (1),
(2), and (3) describes adequately silver cementation only in
the low cyanide regimen. For the high cyanide regimen, the
mechanism suggested by the above results consists, first of
all, of the production of H2 at the zinc–aqueous solution
interface according to the following electrochemical reac-
tions:
Zn0 + 4CN− → Zn(CN)2− −
4 + 2e , (7a)
2H2 O + 2e− → 2OH− + H2 , (7b)
Zn0 + 4CN− + 2H2 O → Zn(CN)2−
4 + 2OH− + H2 . (7c)
The overall Reaction (7c) increases the pH around the
zinc particles leading to the formation of a high-alkalinity
microenvironment. Hydrogen is then transported either by
diffusion or through gas microbubbles to the inner silver–
cyanide interface. It then continues its diffusion through the
pores of the silver shell until it finally reduces silver–cyano
 G. Viramontes Gamboa et al. / Journal of Colloid and Interface Science 282 (2005) 408–414
species on the outer silver–aqueous solution interface. The
reduction reaction on this interface may be either a simple
redox reaction given by
1 These novel results demonstrate that some electrochem-
Ag(CN)− 2 + 2 H2 → Ag + 2CN + H
0 − + (8)
or an electrochemical scheme in which hydrogen oxidation
and silver reduction take place at physically separated sites
as follows
1 4. Conclusions
H2 → H+ + e − , (9a)
2
Ag(CN)− − −
2 + e → Ag + 2CN ,
0 (9b)
1 powder depend on the cyanide concentration. At low free
Ag(CN)−
2 + H2 → Ag0 + 2CN− + H+ . (9c)
2
Both Reactions (8) and (9c) leads to the formation of
a less-alkaline microenvironment. The chemical species in-
volved in those reactions are adsorbed at the outer silver–
aqueous solution interface. Adding Reactions (7c) and either
(8) or (9c) leads to the overall silver cementation stoichiom-
etry for high cyanide concentrations given by Reaction (6).
Accordingly, the ε = 1 relation originates because the areas
for zinc dissolution and silver deposition are not electrically
but electrolytically connected. Maybe the role of hydrogen
microbubbles is to separate the zinc powder particles from
the silver shell.
The two different mechanisms of silver deposition at
low and high cyanide concentration can be accounted for
by the stability of Zn(OH)2 and its relationship to the
rate-determining steps of the cementation process. At low
cyanide concentration and high pH, Zn(OH)2 is highly sta-
ble and it has been found that it coats the surface of zinc
[1,4,6,16]. Under these conditions the rate-determining step
is the zinc oxidation [17]. Thus, silver–cyano species diffuse
from the bulk solution to the zinc–aqueous solution interface
where they are cathodically reduced. Then the cementation
process follows a shrinking core behavior as observed in
Fig. 4a, which shows the cemented silver growing toward
the center of the zinc particle.
At high cyanide concentration, zinc–cyano complex
species are more stable than Zn(OH)2 [6,16]. Under these
conditions the cementation process has been reported to be
controlled by diffusion through the boundary layer [4,6],
which agrees well with the dense-branching morphology of
the silver deposit [1] and a first-order rate for the cemen-
tation Reaction [6]. When cementation starts, silver–cyano
species are first reduced at the zinc–aqueous solution inter-
face forming the initial silver layer, which is readily elec-
trically charged driving the silver–cyano species adsorbed
at this interface to be discharged. So the diffusion control
through the boundary layer is established and the reduction
of silver–cyano species will take place at the silver–aqueous
solution interface making the deposit grow outward. For this
to occur in the absence of an electrical contact between the
silver layer and the zinc particle, the reducing species needs
to have a diffusion coefficient higher than that of Ag(CN)− 2,
413
which is 1.5 × 10−5 cm2 /s [6]. Molecular hydrogen meets
this requirement as it is smaller in size in comparison with
that of Ag(CN)− 2.
ical methods, such as Evans diagrams, should be used with
a lot of precautions to carry out silver cementation on zinc
studies particularly at high cyanide concentrations.
The chemical routes and morphological patterns present
in the cementation of silver from cyanide solutions with zinc
cyanide concentrations an electrochemical process taking
place on the zinc particles describes well experimental ob-
servations. For high free cyanide concentrations, like those
commonly used in plant operations, zinc oxidation and silver
reduction reactions take place on different, non-electrically
connected, interfaces. Under this last condition, the absence
of contact between both metals causes the reduction of the
efficiency of zinc to recover silver, exactly by one half of its
theoretical maximum.
Acknowledgments
This work has been partially supported by the Consejo
Nacional de Ciencia y Tecnología, México, Grants G29589E
and ER026 Materiales Biomoleculares, and by Centro de
Investigación y Desarrollo Tecnológico de Servicios Indus-
triales Peñoles. The authors thank Professor Bernardo José
Luis Arauz Lara for the assistance in the use of the equip-
ment at the Laboratorio de Fluidos Complejos, Instituto de
Física, Universidad Autónoma de San Luis Potosí. Thanks
to Dr. Miguel Angel Vidal for use of the mass spectrometer,
Instituto de Investigación en Comunicaciones Opticas, from
the same University, and for helpful discussions.
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