Hydrometallurgy 87 (2007) 51 – 57

www.elsevier.com/locate/hydromet

Process development for the separation and recovery of copper

from sulphate leach liquors of synthetic Cu–Ni–Co–Fe
matte using LIX 84 and LIX 973N
B. Ramachandra Reddy a,b,⁎, Kyung Ho Park b , D. Mohapatra b
a
Inorganic Chemistry Division, Indian Institute of Chemical Technology (CSIR), Hyderabad - 500 007, India
b
Minerals and Materials Processing Division, Korea Institute of Geoscience and Mineral Resources (KIGAM),
Daejeon 305-350, Republic of Korea

Received 27 August 2006; received in revised form 19 January 2007; accepted 26 January 2007
Available online 8 February 2007

Abstract

Solvent extraction separation and recovery of copper from liquors from sulphate leaching of synthetic Cu–Ni–Co–Fe matte
using oxime based extractants such as LIX 84 and LIX 973N in kerosene was studied. Parameters such as feed pH, extractant
concentration, phase ratio, counter current extraction and stripping were optimized. Influence of feed pH on copper extraction
indicates that leach liquor acidity was adequate to achieve maximum extraction. Comparison of the extraction behavior of
extractants for copper at 40 vol.% concentrations showed 10% more extraction with LIX 973N. Extraction isotherm data with
40 vol.% LIX extractants (barren of copper) at unit phase ratio indicated 3 stages of extraction with LIX 84 and 2 stages of
extraction with LIX 973N, are necessary to achieve N 95–99% copper extraction. The co-extraction of Ni, Co and Fe was b 2 mg/L.
Stripping of copper from loaded organic phase at unit phase ratio using a synthetic spent electrolyte (SE) solution containing 35 g/L
Cu and 180 g/L H2SO4 from Cu-LIX 84 loaded organic (LO) was ∼ 81%, whereas from Cu-LIX 973N LO, it was ∼ 10%. Two
stages of stripping of copper from LIX 84-LO at O/A ratio of 1.3 with SE indicated 85% stripping. Recycle of spent organic for
further use in copper extraction circuit showed a decrease in efficiency by ∼ 3–4%. Semi-continuous countercurrent extraction
(∼ 96%)–stripping (∼ 85%) studies for 4 cycles on lab scale and bench scale mixer settler equipment for 30 h of operation
confirmed almost similar extraction–stripping percentages with high purity copper sulphate solution.
© 2007 Elsevier B.V. All rights reserved.

Keywords: Process development; Copper recovery; Sulphate leach liquor; Cu–Ni–Co–Fe matte; LIX 84; Bench scale run

1. Introduction refining. Leaching/solvent extraction (SX)/electrowin-

Copper is primarily produced from sulphide ores/
concentrates by pyrometallurgical smelting and electro-
⁎ Corresponding author. Minerals and Materials Processing Divi-
sion, Korea Institute of Geoscience and Mineral Resources (KIGAM),
Daejeon 305-350, Republic of Korea.
E-mail address: brcreddy_iict@yahoo.com
(B. Ramachandra Reddy).
0304-386X/$ - see front matter © 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.hydromet.2007.01.004
ning (EW) has been a commercial process since 1968
for oxide ores and since the mid 70s for mixed oxide–
sulfide ores. Today about 30% of world copper is pro-
duced by acid leach (AL)–SX–EW technology (Cox,
2004). Presently, two processes are at the demonstration
plant stage for the recovery of Cu, Ni and Co from
nickel concentrate by an oxidative pressure leach-SX
technique (Palmer and Johnson, 2005; Kelly, 2006). In
these copper was separated using Acorga M5460
52 B. Ramachandra Reddy et al. / Hydrometallurgy 87 (2007) 51–57

extractant dissolved in Shellsol D70. Further, the grow-

ing demand for high purity metals and the rapid dep-
letion of land based ores have necessitated the need for
exploitation of alternative sources to meet the future
demands. One such source appears to be the vast oceans
which are claimed to contain millions of tons of re-
sources containing copper, nickel and cobalt (N 2%) in
the form of polymetallic manganese nodules (4–5 km
depth), polymetallic sulphide deposits containing Ag,
Ni, Co (1–2 km depth) and cobalt rich ferromanganese
crusts (0.4–4 km depth) (Rona, 2003).
Worldwide efforts are in progress for the last three
decades to develop processes based on pyrometallur-
gical, pyro–hydrometallurgical or hydrometallurgical
routes to recover three (Cu, Ni, Co) or four (Cu, Ni,
Co, Mn) metals from manganese nodules (Jung, 1993;
Fuerstenau and Han, 1977, 1983; Haynes et al., 1987).
Some of the processes such as gaseous reduction –
ammoniacal leach, cupric ammoniacal leach, high tem-
perature–pressure sulphuric acid leach and smelting –
sulphuric acid leach, tried on a pilot plant scale for
manganese nodules processing are similar to the cur-
rently practiced technology for nickel laterite ore (Jung,
1993). The research team of minerals and materials
processing division of KIGAM supported by the Ko-
rean Government has been working on processing Pa-
cific Ocean manganese nodules for the recovery of
valuable metals in the form of a Cu–Ni–Co–Fe matte
by a reductive roasting and smelting technique (Nam Fig. 1. General flowsheet of the process for the treatment of manganese
et al., 2003). Matte was subjected to oxidative pressure nodules.
leaching with dilute sulphuric acid to selectively extract
copper, nickel and cobalt leaving Fe in the residue
(Nam et al., 2004). A general flowsheet of the process aldoximes. However, mixtures of oximes have shown
for the treatment and recovery of copper, nickel and advantages over separate groups (Kordosky et al., 1983).
cobalt from manganese nodules by pyro–hydrometal- Among the LIX reagents, LIX 84 has been applied
lurgical method is presented in Fig. 1. extensively for the recovery of copper commercially
Leaching, solvent extraction, electrowinning pro- (Cox, 2004) and in several studies for the removal/
cesses have been increasingly important to concentrate, recovery of copper from other metal containing sources
purify and separate metal ions. The largest commercial (Cox, 2004; Sahu et al., 2004; Parija et al., 1998). Studies
application of these processes is in the copper industry on LIX 973N are few, limited to copper extraction from
(Kordosky, 1992). A large number of commercial cop- ammoniacal/ammonium carbonate medium (Alguacil,
per SX/EW plants were successfully commissioned all 1999; Alguacil and Navarro, 2002). In our recent studies,
over the world in the last three decades (Davenport et al., LIX 84-I has been applied for the separation of Cu, Ni
2002) employing copper selective hydroxyoxime based and Zn from sulphate solutions (Ramachandra Reddy
extractants (Szymanowski, 1993; Ritcey and Ashbrook, and Neela Priya, 2004), recovery of Ni from ammonium
1979; Fisher and Notebaat, 1983; Kordosky et al., 1983; sulphate medium (Parija and Bhaskara Sarma, 2000) and
Cox, 2004). The extractants used are either in pure form extraction studies of Zr/Hf from acidic chloride solutions
with/without modifier, or a mixture of two reagents to (Ramachandra Reddy et al., 2004; Ramachandra Reddy
improve the kinetics of extraction and stripping of cop- and Rajesh Kumar, 2005).
per (MCT Redbook, 1998). Only two classes of extrac- The aim of the present study is to optimize conditions
tants have gained commercial acceptance as reagents for on a lab scale for the solvent extraction separation and
SX of Cu from acidic leach solutions: ketoximes and recovery of copper from concentrated sulphate leach
 B. Ramachandra Reddy et al. / Hydrometallurgy 87 (2007) 51–57
liquor obtained by the dilute sulphuric acid pressure
leaching of synthetic Cu–Ni–Co–Fe matte similar to the
matte generated by the reduction roasting and smelting
of Pacific Ocean nodules (Nam et al., 2003) using LIX
84 and LIX 973N as the extractants. Stripping of copper
from loaded extractant was carried out with a synthetic
spent electrolyte (SE) to generate pregnant electrolyte
(PE) suitable for producing copper metal by electro-
winning. Process parameters such as extractant concen-
tration, feed pH, organic to aqueous phase ratio, counter
current extraction and stripping simulation and recycle of
extractant for reuse in continuous copper extraction circuit
were carried out to determine the suitability of these
extractants for separation of copper from LL containing
Cu, Ni, Co and Fe. Based on the results, a flowsheet of the
process was proposed. Finally, lab scale conditions were
tested on bench scale continuous mixer settler equipment.
2. Experimental
2.1. Apparatus
A Varian model SpectrAA 400 Atomic Absorption
Spectrophotometer (AAS) and an Orion expandable ion
analyzer EA 920 equipment were used for the deter-
mination of metal concentrations and pH of the aqueous
phase.
2.2. Reagents
The typical composition of leach liquor generated
from synthetic Cu–Ni–Co–Fe matte leaching (10 vol.%
H2SO4, 5% solids to liquid ratio, 10 kg/cm2 pressure,
1 h) contains copper – 10.68 g/L, nickel – 16.8 g/L,
cobalt – 1.85 g/L, iron – 0.07 g/L at pH = 2.2. The
commercial oxime based extractants LIX 84 (2-hydroxy-
5-nonylacetophenoneoxime in a mixture with a small
amount of 5-dodecyl-salicylaldoxime and a high flash
point hydrocarbon diluent) and LIX 973N (an approximate
7/3 mixture of 5-nonylsalicylaldoxime and 2-hydroxy-5-
nonylacetophenoneoxime in a high flash point hydrocar-
bon diluent) supplied by Cognis, Ireland were used as such
without any purification. Extra pure kerosene supplied by
Junsei Chemical Co, Japan was used as the diluent.
Shakeout experiments were carried out in separating
funnels. All the other chemicals were Analar grade.
2.3. Solvent extraction procedure
Suitable volumes of aqueous and organic phases
were contacted for 5 min (initial experiments showed
that equilibrium was reached within 1 min) in separating
53
funnels. The phases were separated and the metal con-
centration in the aqueous phase determined by AAS.
The loaded organic (LO) phases were stripped three
times with 2 M HCl wherever necessary, and the com-
bined strip solutions analysed by AAS. All the experi-
ments were carried out at room temperature (25 ± 1 °C).
The distribution ratio, D, was calculated as the concen-
tration of metal present in the organic phase to that part
in the aqueous phase at equilibrium.
Continuous mixer settler runs for copper extraction–
stripping were conducted for 30 h. Each mixer settler
unit, in which the volumes of the mixer and the settler
were 200 and 600 mL, respectively, was counter cur-
rently connected and flow rates of aqueous and organic
phases were maintained according to lab scale data
(extraction: O/A = 1, 3 stages; stripping: O/A = 1.5, 2
stages). Samples from extraction and stripping circuits
such as raffinate, loaded organic and spent organic were
collected for estimation of copper extraction–stripping
percentages.
3. Results and discussion
3.1. Variation of feed pH and extractant concentration
Initial experiments on single stage extraction of cop-
per from leach liquor (pH: 2.2) without pH adjustment at
unit phase ratio with 30 vol.% LIX 84 and LIX 973N
dissolved in kerosene indicated about 75 and 93%
extraction, respectively. In order to improve the
percentage extraction of copper, leach liquor pH was
adjusted to different values from 1.45 to 3.1 and
extraction tests were carried out with 30 and 40 vol.%
Fig. 2. Effect of initial pH of leach liquor on copper extraction.
Organic: 30 and 40 vol.% LIX 84/LIX 973N in kerosene.
54 B. Ramachandra Reddy et al. / Hydrometallurgy 87 (2007) 51–57

tractants (barren of copper), extraction was carried out at

varying O/A ratios from 0.20 to 10 (Fig. 3). In case of LIX
973N, the shape of extraction isotherm indicates high
distribution coefficients. In case of LIX 84, the curve
represents S-shaped isotherm and it is apparent from the
McCabe–Thiele plots that the raffinate would always be
left with some copper (Ritcey and Ashbrook, 1979). In the
present study with 40 vol.% LIX 84 at O/A ratio of 1, the
plot indicates about 0.5 g/L Cu in the raffinate after 3
extraction stages, whereas LIX 973 is almost quantitative
under similar extraction conditions. Analysis of organic
phases indicated 1–2 mg/L co-extraction of Ni, Co, Fe,
indicating clear separation of copper from other metals.

3.3. Counter current batch simulation studies for

Fig. 3. McCabe–Theile plot for copper extraction. Organic: 40 vol.%
LIX 84/LIX 973N in kerosene.
LIX 84 and LIX 973N (Fig. 2). In the case of 30 and
40 vol.% LIX 84, an increase of the leach liquor (LL)
pH up to 2.2 increases the percentage extraction of
copper from 67 to 75 and 77 to 84% respectively,
higher pH showed no significant improvement. With
LIX 973N, the increase in copper extraction for 30
and 40 vol.% solutions was from 90 to 94 and 94 to
96%, respectively. The corresponding change in equi-
librium pH was from 0.7 to 0.9. The results further
indicate that the initial pH of 2.2 was adequate to
achieve maximum percentage extraction of copper and
further experiments were carried out without any pH
adjustment.
3.2. Extraction isotherm of copper
To find out the theoretical number of stages and
possibility of enriching the copper concentration in the
loaded organic phase during extraction stage, the
extraction isotherm was obtained. Using 40 vol.% ex-
copper extraction
Based on the McCabe–Thiele plot, a three stage
counter current extraction simulation (CCES) test was
carried out at O/A phase ratio of unity using 40 vol.% LIX
84 barren of copper. The raffinate contained 70 mg/L of
copper corresponding to a copper extraction efficiency of
99% (Table 1). Using 40 vol.% LIX 973N barren of
copper, a two CCES test under similar conditions resulted
in a raffinate containing 9 mg/L of copper corresponding
to an extraction efficiency of 99.9%. The co-extraction of
Ni, Co and Fe was b 2 mg/L.
3.4. Variation of phase ratio on stripping of copper
from loaded organic
A sufficient quantity of loaded organic phase
(Cu: 10.61g/L for LIX 84 and 10.67 g/L for LIX 973N)
was generated for carrying out the copper stripping
studies with a spent electrolyte containing 35 g/L Cu
and 180 g/L H2SO4. Initial tests on stripping kinetics of
copper from Cu-LIX 84 with spent electrolyte for 0.5,
1, 2, 3 and 5 min contact periods showed 76.1, 79.0,
80.5, 80.3 and 80.4% stripping, respectively, indicating

Table 1
Analysis of inlet and outlet streams during counter current extraction simulation of copper
Stream pH 40 vol.% LIX 84; pH 40 vol.% LIX 973N
3 stage C–C extraction 2 stage C–C extraction
[Cu], g/L Cu extraction, % [Cu], g/L Cu extraction, %
Feed 2.2 10.68 – 2.2 10.68 –
Organic solvent – – – – – –
Raffinate 0.9 0.07 99.3 0.82 0.009 99.9
Stage 2 raffinate 0.92 0.92 95.5 – – –
Stage 1 raffinate 1.15 2.24 79.0 0.84 0.246 97.7
Loaded organic (LO) – 10.61 – 10.671 –
Impurities in LO (mg/L) – Ni – 0.5; Co, Fe – 0.8 Ni – 1.0; Co – 0.7; Fe – 0.9
 B. Ramachandra Reddy et al. / Hydrometallurgy 87 (2007) 51–57 55

Table 2
Effect of acid concentration and phase ratio on the stripping of copper from loaded organic using depleted electrolyte containing 35 g/L Cu and
H2SO4
40 vol.% LIX 84 40 vol.% LIX 973N
a
Phase ratio (A:O) [H2SO4], g/L Cu in LO, g/L Cu in SO, g/L % Cu stripping Cu in LO, g/Lb Cu in SO, g/L % Cu stripping
1:1 220 10.61 1.61 84.7 10.671 9.0 15.4
1:1 200 – 1.91 82.0 – 9.15 13.8
1:1 180 – 2.07 80.5 – 9.47 10.7
1:1.3 180 – 1.96 81.5 – 9.61 9.4
1:1.5 180 – 2.10 80.2 – 9.90 6.7
1.5:1 180 – 1.80 83.0 – 9.54 10.1
2.0:1 180 – 1.70 84.0 – 9.86 7.1

2 min contact was sufficient to achieve equilibrium. Since quantitative copper stripping, semi-continuous counter
the objective was to obtain a pregnant electrolyte current tests were carried out (2 cycle extraction using
containing about 50 g/L copper and 157 g/L H2SO4 1st cycle SO and so on) for 4 cycles (extraction: O/A = 1;
suitable for copper electrowinning with a copper dep- stripping: O/A = 1.5) with a view to optimize the phase
letion of 15 g/L, stripping studies were carried out using ratio and number of cycles required to generate electro-
spent electrolyte containing 35 g/L copper and varying lyte containing ∼ 50 g/L copper by striping using dep-
concentrations of H2SO4 from 180 to 220 g/L and leted electrolyte (35 g/L copper and 180 g/L H2SO4).
different phase ratios in order to determine the percentage
stripping and possible enrichment of copper (Table 2). In
the case of Cu-LIX 84 increasing acid concentration from
180 to 220 g/L at unity phase ratio showed an increase in
stripping of about 4%. Increasing the A/O phase ratio
from 1 to 2 indicated a similar increase in stripping. These
results indicate that about 3 stages of stripping are
necessary to theoretically strip more than 99% copper
from LO using 180 g/L acid at unity phase ratio. The
stripping of copper from Cu-LIX 973N was in the range
from 7 to 15%, indicating the non-suitability of this
extractant under the present stripping conditions.

3.5. Counter current stripping simulation for copper

from loaded organic

Considering copper stripping of 81.5% from the

loaded organic in a single stage with SE (35 g/L Cu and
180 g/L H2SO4) at O/A phase ratio of 1.3, a three stage
counter current stripping would give theoretically ∼ 99%
stripping. Accordingly, a 3 stage simulation was carried
out, the first two stages stripped ∼ 88.5% but three only
gave ∼ 90% stripping. Similar incomplete stripping of
copper from loaded LIX 84 and LIX 64N with spent
electrolyte has been reported in literature (Ritcey, 1979;
MCT Redbook, 1998).

3.6. Semi-continuous counter current extraction and

stripping tests for copper recovery from leach liquor
Fig. 4. Semi-continuous counter current lab and mixer settler results
As the stripping tests of copper from loaded organic for copper recovery with 40 vol.% LIX 84. Open symbol – lab data;
phase reported in the previous section did not yield closed symbol – continuous mixer settler.
56 B. Ramachandra Reddy et al. / Hydrometallurgy 87 (2007) 51–57
Fig. 5. Effect of feed pH vs. percent of metal precipitation. Conditions:
50% NaOH solution, 75 °C, 1 h.
Results of these tests are presented in Fig. 4 (open
symbols). It can be seen that the stripping of copper at
O/A ratio of 1.5 for 4 cycles of semi-continuous ex-
traction–stripping decreased in efficiency by about 2 to
3%. The extraction (∼ 96%) and stripping (∼ 84%)
remains almost the same after second cycle and the
generated pregnant electrolyte contains about 50 g/L
copper and 157 g/L H2SO4, which is suitable for pro-
duction of high grade copper metal with a purity of
N99.98%.
The raffinate after copper extraction contained about
0.4 g/L copper, 0.07 g/L iron, 16.8 g/L nickel and
Fig. 6. Flowsheet of the process for the separation and recovery of copper from sulphate leach liquors of synthetic Cu–Ni–Co–Fe matte.
1.85 g/L cobalt at a pH of ∼ 1.0. This solution would
require processing to remove Cu and Fe before cobalt–
nickel separation. Results on impurities removal from
raffinate adjusted to different pH values in the range
from 5.3 to 7.7 with dilute alkali solution (50 wt.%)
indicated quantitative removal of Cu and Fe around
7.5 pH where the loss of Ni and Co was 2.2–2.7%
(Fig. 5). Based on the results, a process flowsheet for the
separation and recovery of copper is presented in Fig. 6.
3.7. Bench scale mixer settler runs
A bench scale mixer settler run was conducted under
the optimum lab scale conditions (extraction: O/A = 1, 3
stages, 40% LIX 84I containing 1.7 to 1.9 g/L Cu, i.e.
SO from stripping stage; stripping: O/A = 1.5, 2 stages,
SE containing 35 g/L Cu and 180 g/L H2SO4) for 30 h.
The stripped organic phase was recycled back to the
extraction stage continuously during the bench scale
run. Loaded organic, raffinate, and stripped organic
samples were collected to determine the extraction and
stripping efficiencies of copper. The results of these tests
are presented in Fig. 4 (closed symbols). The extraction
and stripping efficiencies of copper were ∼ 90 to 92%
and ∼ 85 to 87% respectively, indicating agreement
with laboratory data within ± 3%.
4. Conclusions
Extraction of copper from sulphate liquor of syn-
thetic Cu–Ni–Co–Fe matte using 40 vol.% LIX 84 and
LIX 973N in kerosene at unit phase ratio indicated
 B. Ramachandra Reddy et al. / Hydrometallurgy 87 (2007) 51–57
percentage extraction of 83 and 95% respectively. Strip-
ping using spent electrolyte (35 g/L Cu and 180 g/L
H2SO4) in a single stage at unity phase ratio was ∼ 81
and 10% for LIX 84 and LIX 973N respectively. Two
stage extraction of copper with 40% LIX 84 (i.e. SO
containing ∼ 1.75–1.85 g/L Cu) gave about 97% copper
extraction. Three/two stage stripping of copper from
loaded organic at O/A ratio of 1.3 gave about 90–88.5%
stripping, resulting in b15 g/L Cu enrichment in preg-
nant electrolyte solution. As a result, extraction and
stripping conditions were established at O/A ratio of 1.5
in lab scale experiments, which resulted equilibrium
conditions of extraction (∼ 96 ± 1%) after second cycle
onwards. Bench scale continuous mixer settler experi-
ments confirmed the lab scale data with small variations
in percentage copper extraction and stripping. Finally,
flowsheet of the process is demonstrated.
Acknowledgements
BRR express sincere thanks to Dr. J. S. Yadav,
Director, Indian Institute of Chemical Technology (IICT),
Hyderabad, India for permission on deputation and to
Korea Federation of Technology and Science (KOFTS),
Seoul, Korea for the financial support under Brain Pool
Program.
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