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Dissolution Kinetics of Malachite in Ammonia/Ammonium Carbonate

Leaching

Article  in  Hydrometallurgy · January 2005

DOI: 10.1016/j.hydromet.2004.09.006

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 Hydrometallurgy 76 (2005) 55 – 62
www.elsevier.com/locate/hydromet

Dissolution kinetics of malachite in ammonia/ammonium

carbonate leaching
D. Bingfla, M. Canbazoğlub,*, S. Aydoğanc
a
Department of Mining Engineering, DumlupV nar University, Kütahya, Turkey
b
Department of Mining Engineering, Cumhuriyet University, Sivas, Turkey
c
Department of Mining Engineering, Selçuk University, Konya, Turkey
Received 12 June 2004; received in revised form 3 September 2004; accepted 10 September 2004

Abstract

The leaching of oxide copper ore containing malachite, which is the unique copper mineral in the ore, by aqueous
ammonia solution has been studied. The effect of leaching time, ammonium hydroxide, and ammonium carbonate
concentration, pH, [NH3]/[NH4+] ratio, stirring speed, solid/liquid ratio, particle size, and temperature were investigated. The
main important parameters in ammonia leaching of malachite ore are determined as leaching time, ammonia/ammonium
concentration ratio, pH, solid/liquid ratio, leaching temperature, and particle size. Optimum leaching conditions from
malachite ore by ammonia/ammonium carbonate solution are found as ammonia/ammonium carbonate concentrations: 5 M
NH4OH+0.3 M (NH4)2CO3; solid/liquid ratio: 1:10 g/mL; leaching times: 120 min; stirring speed: 300 rpm; leaching
temperature: 25 8C; particle size finer than 450 Am. More than 98% of copper was effectively recovered. During the leaching,
copper dissolves as in the form of Cu(NH3)4+2 complex ion, whereas gangue minerals do not react with ammonia. It was
determined that interface transfer and diffusion across the product layer control the leaching process. The activation energy for
dissolution was found to be 15 kJ mol
1.
D 2004 Elsevier B.V. All rights reserved.

Keywords: Copper; Malachite; Ammonia; Ammonium carbonate; Leaching; Diffusion

1. Introduction malachite [Cu2(OH)2CO3], tenorite (CuO), and chrys-

Copper oxide minerals containing copper in the
divalent state, such as azurite [Cu3(OH)2(CO3)2],
* Corresponding author.
E-mail address: mcanbaz@cumhuriyet.edu.tr (M. Canbazoğlu).
0304-386X/$ - see front matter D 2004 Elsevier B.V. All rights reserved.
doi:10.1016/j.hydromet.2004.09.006
ocolla (CuSiO3.2H2O), are completely soluble either
in acidic or alkaline medium at room temperature. It
has been very well known that sulfuric acid is the
most usual leaching agent for oxidized copper ore,
and depending on the nature of ore, acid consumption
ranges from 0.4 to 0.7 ton H2SO4 per ton of copper
recovered. The kinetics and the chemistry of mala-
56 D. Bingöl et al. / Hydrometallurgy 76 (2005) 55–62
chite ore leaching in sulfuric acid and extraction of
copper from raffinate by solvent extraction (SX) have
been investigated intensively (Habashi, 1983; Bingöl
and Canbazoğlu, 2004; Hopkins, 1994; Amores et al.,
1997; Navarro and Alguacil, 1999; Barlett, 1992; Ata
et al., 2001).
Sodium hydroxide, lime, and ammonia are the
most common alkaline reagents used. Ammonia
leaching was first used at the Kennecott Plant, Alaska,
because copper ore contains carbonates in limestone–
dolomite gangue which are acid soluble, consequently
increasing the acid consumption (Habashi, 1970,1983;
Alguacil, 1999). Being more selective, less corrosive
and lowering reagent consumption for calcareous
carbonate gangue are the main advantages of the
alkaline leaching over acid leaching. As it is applied
by the Arbiter process, the raffinate is treated with
lime to regenerate ammonia and to produce disposable
Gypsum (CaSO4d 2H2O) (Kuhn et al., 1974).
A large number of leaching systems in which
complex ions are formed between the metal cation
and complexing species in solutions are extensively
utilized. Ammonium hydroxide is commonly used in
cobalt, nickel, and copper industries due to the
formation of stable metal amine complexes. Com-
plexing ligand includes ammonia and attaches to
metal ion through reactive nitrogen-containing group,
leading to higher solubility in most cases (Forward
and Peters, 1985).
Malachite dissolves in NH4OH/(NH4)2CO3 solu-
tions by forming a stable copper (II) tetra ammine
complex. The ammonia leaching reaction for mala-
chite is defined as:
Cu2 ðOHÞ2 CO3 þ 6NH4 OH þ ðNH4 Þ2 CO3
Y2CuðNH3 Þ4 CO3 þ 8H2 O ð1Þ
A study performed by Oudenne and Olson (1983)
on leaching kinetics of malachite in ammonium
carbonate solution reveals that two stages of reaction
are found. In Stage I, the initial dissolution of
malachite proceeds rapidly, but after about 10% of
reaction is reached, the rate decreases by surface
blockage due to the presence of a needle-structured
intermediate phase, most likely Cu(OH)2. Subse-
quently, malachite and the intermediate phase dissolve
simultaneously. In Stage II, after 90% of reaction is
completed, essentially all of the malachite dissolves,
and only the intermediate remains that dissolves in
Stage II. The rate equations were defined as
1
(1
X)1/3=k 1t for Stage I, and 1
(1
X)1/2=k 2t
for Stage II (where X is the reacted fraction of the
solid, k 1 and k 2 are rate constant, and t is leaching
time). The activation energies were 64 and 75 kJ
mol
1 for Stage I and Stage II, respectively. A kinetic
study performed by Künkül et al. (1994) on leaching
of malachite in ammonia–ammonium carbonate sol-
utions shows that the leaching process was controlled
by diffusion through the ash layer, which is the
insoluble inert gangue material consisted of mainly
SiO2, around the shrinking unreacted core, the integral
rate equation was 1
3(1
X)2/3+2(1
X)=kt. Activa-
tion energy for the leaching process was found to be
22 kJ mol
1. A recent study by Ekmekyapar and Oya
(2003), investigating the ammonium chloride leaching
of malachite, shows that the dissolution rate was
controlled by mixture kinetics. The mathematical
model was proposed to represent the reaction kinetics
is 1
2(1
X)1/3+(1
X)2/3=kt. The activation energy
for the dissolution reaction of malachite was calcu-
lated as 71 kJ mol
1.
The aim of this study is to investigate and discuss
the leaching kinetics and dissolution parameters of
malachite in ammonia/ammonium carbonate solutions.
2. Experimentals
2.1. Materials
Oxidized copper ore was used for leaching experi-
ments. Mineralogical analyses, performed using
Rigaku DMAX IIIC model X-ray diffractometer using
CuKa radiation at 35 kV and 15 mA indicated that
malachite, pyroxene group minerals, quartz, goethite,
and magnetite are the major mineral phase. Typical
chemical analysis of the sample is presented in Table
1. Copper, iron, nickel, cobalt, and chromium content
of the ore sample were determined by Atomic
Table 1
Typical chemical analysis of the copper oxide ore
Component (%)
Cu Fe Ni Co Cr S C SiO2
28.4 15.7 0.044 0.010 0.019 0.10 2.72 15.3
 D. Bingöl et al. / Hydrometallurgy 76 (2005) 55–62
Absorption Spectrophotometer (AAS). Sulfur and
carbon content were determined by LECO-444 SC
analyzer. Quartz content was determined by classical
digestion with HF method. It is worth pointing out
that carbon content originates only from malachite
carbonate and sulfur originates from base metal
sulfides present in the ore.
The ore was crushed, ground, and then sieved
using standard test sieves to obtain desired particle
size fractions for the leaching experiments. The
experiments in which the effects of ammonia/ammo-
nium carbonate concentration and solid/liquid ratio
were investigated were carried out with the ore sample
whose 80% is finer than 650 Am. The experiments in
which the effects of temperature was investigated
were performed using 450+250 Am size ore. pH
measurements were performed using HANNA 8521
pH-meter in the solutions obtained before and after
the leaching experiments.
2.2. Method
A Pyrex beaker (600 mL) was used as a leaching
reactor. It was closed by a rubber cover. On the cover,
there are three holes for taking samples from leach
solution, mechanical Teflon stirrer, and pH electrode.
The temperature of the leach solution in the reactor
was provided by a thermostatically controlled water
bath. Required amount of ore was added into the
agitated NH4OH/(NH4)2CO3 solution of given con-
centration at the given temperature. After a specific
time, about 5 mL of leaching solution sample was
withdrawn from the reactor, and fresh 5 mL of
NH4OH/(NH4)2CO3 solution was immediately added
to leaching reactor. The sample solution was analyzed
for copper by AAS. Filtration was made after each
leaching experiment. The weight loss in the solid
phase occurred after leaching was calculated accord-
ing to difference between the weight of solids before
and after the leaching.
3. Results
3.1. Effect of ammonia concentration
Prior to the experiments investigating the effect of
NH4OH together with (NH4)2CO3 at different concen-
57
trations, the effects of NH4OH and (NH4)2CO3 on the
dissolution of malachite were investigated separately.
The graphs giving the results for the copper recovery
and also the pH of ammonia and ammonium carbonate
solutions are given in Figs. 1 and 2. The copper
recovery increases either with ammonia or ammonium
carbonate concentration increases. The increase is fast
up to 5 M NH4OH, then dissolution rate decreases.
However, the increase attends at investigated intervals
for (NH4)2CO3. For example, the malachite dissolution
was 72% at 13.4 M NH4OH, while it was 7% at 1 M
NH4OH (Fig. 1). On the other hand, the copper
recovery reaches to 36% for 2 M (NH4)2CO3 while it
is 2% in 0.1 M (NH4)2CO3 (Fig. 2).
pH of leaching solution increases with increase in
NH 4OH concentration, while it decreases with
increasing (NH 4 ) 2 CO 3 concentration. The pH
increases from 11.8 to 12.5, depending on the increase
of NH4OH concentration from 1 to 13.4 M, while by
increasing (NH4)2CO3 concentration from 0.1 to 2 M,
pH decreases from 9 to 8.5.
Copper recoveries for 5, 30, 120, and 140 min of
leaching by NH4OH+(NH4)2CO3 solution are given in
Fig. 3. These results indicate that the copper recoveries
increase with increasing leaching times for each
ammonia/ammonium concentrations [that is, for 5 M
NH4OH+0.3 M (NH4)2CO3 leaching conditions, the
Fig. 1. Effect of NH4OH concentration on the recovery of copper
from the malachite ore and the change in the pH during the leaching
(temperature, 25 8C; particle size, 80%
650 Am; weight of ore,
20 g; solid to liquid ratio, 1/5 g/mL; stirring speed, 250 rpm; time,
180 min).
58 D. Bingöl et al. / Hydrometallurgy 76 (2005) 55–62
Fig. 2. Effect of (NH4)2CO3 concentration on the recovery of copper
from the malachite ore and the change in the pH during the leaching
(temperature, 25 8C; particle size, 80%
650 Am; weight of ore,
20 g; solid to liquid ratio, 1/5 g/mL; stirring speed, 250 rpm; time,
180 min).
copper recovery is 49% at the end of 5 min of leaching,
and it reaches to 80% at the end of 240 min]. The
copper recovery increases with increasing NH4OH
concentration until 5 M NH4OH+0.3 M (NH4)2CO3
concentration with increase in NH4OH concentration.
This increase reaches to 80% at the end of 240 min,
Fig. 3. Effect of NH4OH+(NH4)2CO3 on the recovery of copper
from the malachite ore (temperature, 25 8C; particle size, 80%

650 Am; weight of ore, 20 g; solid to liquid ratio, 1/5 g/mL;
stirring speed, 250 rpm).
while the copper recovery decreases for higher NH4OH
concentrations [that is, the copper recovery for 6 M
NH4OH+0.25 M (NH4)2CO3 solution decreases to
53% at the end of 240 min of leaching]. It seems that 5
M NH4OH+0.3 M (NH4)2CO3 concentration is suit-
able as optimum ammonia/ammonium concentration.
3.2. Effect of leaching time
The effect of leaching time on the dissolution of
malachite was studied. The results are given in Fig. 4.
According to experimental results presented in Fig. 4,
the copper recovery increased with increasing leach-
ing time. At the beginning of leaching, dissolution of
malachite was very fast. After 5 min, 49% copper
recovery was achieved. After 30-min leaching time,
copper recovery increases rather slowly. This value
reached to 80% at the end of 240 min.
3.3. Effect of solid/liquid ratio
The effect of solid/liquid ratio on the dissolution of
malachite was investigated in the range of 1:1–1:10.
The results with the weight loss are presented in Fig. 5.
Liquid volume was kept constant, and the amount of
solid was changed to obtain the desired ratio during the
Fig. 4. Effect of leaching time on the recovery of copper from the
malachite ore (ammonia concentration: 5 M NH4OH + 0.3 M
(NH4)2CO3; temperature, 25 8C; particle size, 80%
650 Am; weight
of ore, 20 g; solid to liquid ratio, 1/5 g/mL; stirring speed, 250 rpm).
 D. Bingöl et al. / Hydrometallurgy 76 (2005) 55–62 59

Table 2
Effect of particle size on recovery of copper and the weight loss
from malachite ore (ammonia concentration: 5 M NH4OH+0.3 M
(NH4)2CO3; temperature, 25 8C; weight of ore, 20 g; solid to liquid
ratio, 1:5; stirring speed, 250 rpm; time, 180 min)
Particle size (mm) Copper recovery (%) Weight loss (%)
+4.760 37.0 18.6

4.760+2.830 54.7 27.6

2.830+2.000 68.1 33.6

2.000+0.841 70.2 34.6

0.841+0.212 75.0 37.1

0.212+0.150 81.0 40.0

0.150+0.100 90.0 44.4

0.100+0.075 95.0 46.9

0.075+0.045 98.5 48.5

0.045 98.9 48.8

dissolution of malachite. The copper recovery was

Fig. 5. Effect of solid to liquid ratio (w/v) on the recovery of copper
from the malachite ore and on the weight loss during the leaching
(ammonia concentration: 5 M NH4OH + 0.3 M (NH4)2CO3; temper-
ature, 25 8C; particle size, 80%
650 Am; stirring speed, 250 rpm;
time, 180 min).
experiments carried out at various solid/liquid ratios.
The copper recovery increased with decrease in the
amount of solid. However, there was no change in
copper recovery at ratios after 1/5. The weight loss
pattern was similar to malachite dissolution.
3.4. Effect of particle size
approximately 2–3% when no stirring was applied at
0–30 min, while it was 54%, 64%, and 65%,
respectively, at 5, 15, 30 min leaching when 350
rpm stirring speed was applied. The same effect of
stirring speed was not observed on iron minerals
dissolution. It can be concluded that this effect occurs
by the increased diffusion rate of ions in leaching
medium with increasing agitation.
3.6. Effect of temperature
The effect of temperature on the dissolution of
malachite was investigated (Fig. 7). Depending on

The effect of particle size on the malachite leaching

with 5 M NH4OH+0.3 M (NH4)2CO3 at 25 8C was
studied. The copper contents of each size fraction
were considered for the copper recovery calculation.
The results are given in Table 2. According to particle
size fractions, the velocity of dissolution and weight
loss increase as the particle size decreases. The copper
recovery was 99% for
45 Am fraction, while it was
37% for
6.73+4.76 mm fraction at 180 min of
leaching. The results indicated that particle size is an
important parameter for leaching.

3.5. Effect of stirring speed

Fig. 6. Effect of stirring speed on the recovery of copper from the
Fig. 6 shows the effect of stirring speed applied in malachite ore (ammonia concentration: 5 M NH4OH + 0.3 M
the range of 170–350 rpm on the dissolution of (NH4)2CO3; temperature, 25 8C; particle size, 80%
650 Am;
malachite. The stirring speed directly affected the weight of ore, 25 g; solid to liquid ratio, 1/10 g/mL).
60 D. Bingöl et al. / Hydrometallurgy 76 (2005) 55–62
Fig. 7. Effect of leaching time on the recovery of copper from the
malachite ore for various temperatures (ammonia concentration: 5
M NH4OH+0.3 M (NH4)2CO3; particle size,
450+250 Am; weight
of ore, 25 g; solid to liquid ratio, 1:10; stirring speed, 300 rpm).
leaching time, the copper recovery increases as
temperature increases. While the recovery after 5
min reached to 48% and 73%, the recovery after
120 min reached 97% and 99% for 15 and 65 8C,
respectively. There is no significant effect of
temperature on copper recovery after 120 min of
leaching.
4. Discussion
XRD analyses of leaching residue obtained after
leaching at optimum conditions show that malachite
completely dissolves, whereas pyroxene group min-
erals, quartz, goethite, and magnetite naturally do not
dissolve. Removal of malachite by dissolution
increases the content of other minerals found in the
ore. Combining the chemical analyses and XRD data,
it was estimated that the ore consists of 49.4%
malachite, 22.6% goethite and magnetite, 27.4%
quartz, and pyroxene group minerals, only with
0.6% unaccounted for by XRD analysis. Depending
on complete dissolution of malachite at the optimum
leaching conditions, goethite and magnetite and the
other minerals report to residue and reach to 49% and
51%, respectively.
NH 4 OH and (NH 4 ) 2 CO 3 solutions are used
together as leaching medium in the leaching oper-
ations of malachite ores. The highest copper recov-
eries and pH value of the ammonia leaching medium
from malachite leaching are given in Table 3. Only
when 5 M NH4OH is used as leaching medium,
maximum copper recovery is about 53% (Fig. 1), and
when 0.3 M (NH4)2CO3 solution is only used, reached
copper recovery remain at about 5% (Fig. 2).
Although when both the ammonia reagents [5 M
NH 4 OH+0.3 M (NH 4 ) 2 CO 3 solution] are used
together, copper recovery reached about 80%. While
13.4 M NH4OH solution is used as leaching medium,
copper recovery could reach to 72%.
Copper recovery is increased using NH4OH/
(NH4)2CO3 buffer solution because the pH of buffer
solution changes slowly during leaching (F0.5), and
this also provides the formation of stable Cu–
ammonia complexes. On the other hand, the pH of
ammonia medium can be put forwarded from the
thermodynamic estimation of Cu(NH3)42+ equilibrium
state (Tozawa et al., 1976; Galitis et al., 1978). The
region where Cu(NH3)42+ complex is stable is defined
as a function of temperature, total ammonia concen-
tration {[NH3]+[NH4+]}, and pH. The same state also
seems for Cu–NH3 system on the Eh-pH diagram. The
optimum pH range for stable copper complex is found
from diagrams between 8.30 and 10.80 that is
consistent with the results given in Table 3. The same
findings are also given in Künkül et al. (1994).
Kinetic evaluation of reactions which occurred
during the ammonia leaching of malachite indicates
that the types of the reactions are not conformed either
with chemical or diffusion kinetic models of dis-
solution. On the other hand, these models are
Table 3
Relationship between pH and recovery in various ammonia leaching
mediums (temperature, 25 8C; particle size, 80%
650 Am; weight
of ore, 20 g; solid to liquid ratio, 1/5 g/mL; stirring speed, 250 rpm;
time, 180 min)
Leaching medium pH Copper recovery (%)
3 M NH4OH+1 M (NH4)2CO3 10.23 64.1
4 M NH4OH+0.5 M (NH4)2CO3 10.36 67.0
5 M NH4OH+0.3 M (NH4)2CO3 10.77 80.0
6 M NH4OH+0.25 M (NH4)2CO3 11.05 66.6
7 M NH4OH+0.35 M (NH4)2CO3 11.02 67.4
13.4 M NH4OH 12.51 72.0
2 M (NH4)2CO3 8.54 36.0
 D. Bingöl et al. / Hydrometallurgy 76 (2005) 55–62
Fig. 8. Plot of 1/3ln (1
X)
[1
(1
X)
1/3] versus t for different
temperatures.
insufficient to explain the reaction of malachite for the
beginning of the dissolution (i.e., 5–10 min) and for
total leaching period studied, because the curves
obtained from these two models were not very
precise. Although a new model, suggested by Wads-
worth and Miller (1979) and Dickinson and Heal
(1999), based on the interface transfer and diffusion
across the product layer both affect the reaction rate, is
sufficient to explain the malachite ammonia leaching.
Equation of this model is given as follows:
1=3lnð1
X Þ
½1
ð1
X Þ
1=3  ¼ kt
where X is the reacted fraction of the malachite, k is
rate constant, and t is leaching time.
The plot of Eq. (2) versus leaching time, t, for
different temperatures is given in Fig. 8. Clearly, the
model fits well to all data sets. Using the fitted k
values, the Arrhenius curve for the dissolution of
malachite ore is given in Fig. 9. The calculated
activation energy for leaching is 15 kJ mol
1.
5. Conclusions
The main important parameters in ammonia leach-
ing of malachite ore are determined as leaching time,
ammonia/ammonium concentration ratio, pH, solid/
61
liquid ratio, leaching temperature, and particle size.
Optimum leaching conditions from malachite ore by
ammonia/ammonium carbonate solution are found as
ammonia/ammonium carbonate concentrations: 5 M
NH4OH+0.3 M (NH4)2CO3, solid/liquid ratio: 1:10 g/
mL; leaching times: 120 min; stirring speed: 300 rpm;
leaching temperature: 25 8C; particle size finer than
450 Am. Under these conditions, copper recovery may
be as high as 98%.
Generally, copper is soluble as amine complexes at
the ammonia leaching, while iron is hydrolyzed to an
insoluble hydrated iron oxide remaining in the leach
residue. This is also an advantage for the copper
extraction step. Cu(II) forms a number of soluble
amine complexes in the ammonia system, and the
most stable one is tetra-amine. Stable pH interval of
Cu(NH3)42+ complex for the Cu–NH3 system on the
Eh-pH diagram is provided with 5 M NH4OH+0.3 M
(NH4)2CO3 solution in this study. Copper dissolved
from malachite is in the form of stable copper
ammonia complexes in solution.
The dissolution kinetics of malachite in ammonia/
ammonium carbonate solution is controlled by the
interface transfer and diffusion across the product
layer both affect the reaction rate. This model
equation is given as 1/3ln(1
X)
[1
(1
X)
1/3]=kt.
The activation energy of the ammonia leaching
reaction was found to be 15 kJ mol
1.
ð2Þ
Fig. 9. The Arrhenius curve obtained for the dissolution of
malachite ore.
62 D. Bingöl et al. / Hydrometallurgy 76 (2005) 55–62
Acknowledgement
Authors are thankful to Prof. Dr. Hqseyin YalçVn
for evaluation of mineralogical analyses and Assoc.
Prof. Dr. Ünal Akdemir for discussion of results.
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