Hydrometallurgy 74 (2004) 277 – 283

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Cd/EX

Solvent extraction of cadmium (II) from sulphate solutions using

TOPS 99, PC 88A, Cyanex 272 and their mixtures
B. Ramachandra Reddy *, D. Neela Priya, J. Rajesh Kumar
Inorganic Chemistry Division, Indian Institute of Chemical Technology (CSIR), Uppal Road, Hyderabad 500 007, India
Received 1 March 2004; received in revised form 2 June 2004; accepted 3 June 2004

Abstract

Extraction of cadmium (II) from sulphate solutions using organophosphorous-based extractants—TOPS 99, PC 88A and
Cyanex 272 has been studied. Percent extraction of cadmium (II) increased with increasing equilibrium pH of the aqueous
phase and extractant concentration. Extraction of Cd (II) by organophosporus extractants involves cation exchange mechanism
with the formation of 1:3 metal to reagent complex. Characterization of the solid complex of cadmium with TOPS 99 by FTIR,
31
P NMR supported metal complex formation with the phosphorus-hydroxyl (P-OH) group. Finally, the extraction behavior and
possible separation of cadmium and nickel from the mixture of metals was studied.
D 2004 Elsevier B.V. All rights reserved.

Keywords: Organophosphorus extractants; Solvent extraction; Cadmium (II); Synergism; Separation

1. Introduction Literature on cadmium solvent extraction, reports

Cadmium and its compounds are toxic and poi-
soning occurs through inhalation and ingestion. In
spite of its toxicity, it is used in different industries
such as electroplating, pigments, synthetic chemicals,
ceramics, metallurgical and photographic products
(Cheremisinoff, 1995). Cadmium is primarily pro-
duced as a byproduct from mining, smelting and
refining of sulphide ore concentrates of Zn. Secondary
cadmium is recovered from spent Ni –Cd batteries.
Hydrometallurgical methods of treating Cd-containing
materials such as Ni – Cd batteries generate leach
liquors containing Cd and Ni as major metals.
* Corresponding author. Tel.: +91-40-27193510; fax: +91-40-
27160921.
E-mail address: brcreddy_iict@yahoo.com
(B. Ramachandra Reddy).
the use of solvating and cation exchange type
extractants. Wassink et al. (2000) studied the extrac-
tion and separation of cadmium and zinc from
nickel and cobalt from chloride and thiocyanate
solutions using aliquat 336 extractant. Gupta et al.
(2001) have reported extraction and recovery of Cd
from HCl medium using Cyanex 923. The organo-
phosphorus-based extractants studied for the extrac-
tion Cd from other metals such as Zn, Ni were
D2EHPA (Casas et al., 1986; Galan et al., 1998),
Cyanex 272, Cyanex 301 and Cyanex 302 (Nayak
et al., 1995; Avila-Rodriguez et al., 1998; Almela
and Elizalde, 1995).
In this paper, we report the solvent extraction
studies of cadmium from sulphate solutions using
the commercial extractants, TOPS 99, PC 88A and
Cyanex 272 and their mixtures. Various parameters
studied include equilibrium pH, extractant and metal

0304-386X/$ - see front matter D 2004 Elsevier B.V. All rights reserved.
doi:10.1016/j.hydromet.2004.06.001
278 B. Ramachandra Reddy et al. / Hydrometallurgy 74 (2004) 277–283
concentration, synergism, different salts, loading ca-
pacity, stripping of cadmium from loaded organic,
extraction from Ni –Cd mixtures and preparation of
cadmium –TOPS 99 solid complex. The results of this
study are important from the environmental point of
view in the treatment and recovery of cadmium from
wastes such as spent batteries/industrial wastewaters.
2. Experimental
2.1. Reagents
Commercial extractant TOPS 99, (an equivalent of
di-(2-ethylhexyl) phosphoric acid, Heavy Water Plant,
Talcher, Orissa, India), PC 88A (2-ethylhexyl phos-
phonic acid mono 2-ethyl hexyl ester, Daihachi,
Japan) and Cyanex 272 (bis (2,4,4-trimethyl pentyl)
phosphinic acid, Cytec, Canada) were used as re-
ceived. Distilled kerosene (bp: 165 – 200 jC) was
used as the diluent. The sodium salts of the extractants
(60% neutralized) were prepared by adding stoichio-
metric amounts of concentrated NaOH solution to the
extractant in kerosene as required. All other chemicals
were Analar grade. Stock solution of cadmium (II)
sulphate (0.5 M) was prepared in distilled water
containing little H2SO4 to prevent hydrolysis of the
metal ion and standardised against 0.05 M EDTA
solution using Eriochrome Black T as indicator
(Vogel, 1962).
2.2. Apparatus
A digital pH meter (Digisun DI 707 model) and
Atomic Absorption Spectrophotometer (AAS) of Per-
kin-Elmer Model A 300 were used for the measure-
ment of pH and metal concentration in the aqueous
phase. The IR spectrum of the solid complex was
recorded using FTIR-Nicolet (USA)-740-spectropho-
tometer. Phosphorous-31 Nuclear magnetic resonance
measurements were carried out with Varian Unity
Inova 500 MHz instrument using H3PO4 (85%) as
the external standard.
2.3. Solvent extraction procedure
Extraction was carried out with 10 mL of the
aqueous solution containing 0.01 M metal and 0.1
M Na2SO4 equilibrated with equal volume of
sodium salts of the extractants in a separating
funnel. The pH of the aqueous phase was adjusted
initially to the desired value by adding dilute
H2SO4/NaOH solution before equilibration. Initial
experiments on contact time showed that 5 min was
sufficient to reach equilibrium. In all the extraction
experiments after equilibrating for 10 min, the two
phases were allowed to separate. The aqueous
phase equilibrium pH was measured and the metal
concentration was analysed by AAS. The concen-
tration of the metal ion in the organic phase was
calculated from the difference between the metal
ion concentration in the aqueous phase before and
after extraction. The distribution coefficient (D) is
taken as the ratio of the concentration of cadmium
in the organic phase to that present in the aqueous
phase at equilibrium.
For determination of the loading capacity of
0.03 M extractants, the loaded organic (LO) phase
was filtered through a 1PS separating paper and a
suitable aliquot was stripped with 2 M HCl,
followed by analysis using AAS. All the experi-
ments were carried out at room temperature
(30 F 1 jC).
2.4. Preparation of Cd-TOPS 99 solid complex
One hundred milliliters of 0.2 M TOPS-99 in
kerosene was taken in a 500-mL beaker and equal
volume of 0.1 M cadmium was added. Both phases
were stirred for 10 min at an equilibrium pH of
f 5.0 and allowed to stand for phase separation. The
raffinate was separated and fresh cadmium metal
solution was added to the loaded organic phase
repeatedly until the organic phase became saturated
with cadmium. After each contact, concentration of
Cd in the raffinate was analysed. When the raffinate
content of Cd is same as the feed, then the LO was
considered to be fully loaded with Cd. The loaded
organic phase was filtered through phase separator
filter paper. Solvent from the LO phase was allowed
to evaporate under suction at around 80 jC to yield
solid complex. This complex was then washed with
50% ethanol to remove traces of TOPS 99, dried
under vacuum and finally in oven maintained at
around 90 jC and stored in a desiccator (Biswas
and Hayat, 2002).
 B. Ramachandra Reddy et al. / Hydrometallurgy 74 (2004) 277–283 279

3. Results and discussion

3.1. Extraction mechanism and species

The extraction of Cd (II) (0.01 M) from aqueous

sulphate solutions was studied in the equilibrium pH
range 3.6 –7.6 using the sodium form of TOPS 99, PC
88A and Cyanex 272 at 0.02, 0.03 and 0.04 M in
kerosene. Percentage extraction of Cd (II) increased

Fig. 2. Plot of log D vs. log [extractant], M. Org.: TOPS 99 (5), PC

88A (o), Cyanex 272 (D); Aq.: 0.01 M Cd (II), 0.1 M Na2SO4.

with increase in the equilibrium pH of the aqueous

phase. The plot of equilibrium pH vs. log D (Fig. 1)
shows that the plots are linear with a slope of 1.0, 0.9
and 1.3 for TOPS 99; 0.8, 0.6 and 0.7 for PC 88A;
0.6, 0.6 and 0.8 for Cyanex 272 with 0.02, 0.03 and
0.04 M extractants, respectively, indicating the ex-
change of 1 mol of H+ ion with 1 mol of Cd (II).
The influence of extractant concentration on the
extraction of Cd (II) (keeping initial pH at 2.85) was
studied in the range 0.01 –0.04 M. The corresponding
change in equilibrium pH was in the range 3.4 –5.9.
Percentage extraction increased steadily with increase
in extractant concentration with the three extractants.
The increase was 4.3% to 85% in case of TOPS 99,
0.5% to 83.4% in case of PC 88A and 1% to 82.2% in
case of Cyanex 272. The plots of log [extractant], M
vs. log D (Fig. 2) are linear with a slope value of f 3
indicating the association of three moles of the extrac-
tant with the extracted species. Correlation of extrac-
tion behavior of Cadmium (II) at 50% extraction using
0.02 M extractant concentration with their pKa values
clearly indicate direct relation with pKa values. The
0.6 corresponding pH1/2 values for TOPS 99, PC 88A and
e=
slop
Cyanex 272 are 4.5, 5.3 and 5.8, respectively, indi-
cating that TOPS 99 as an efficient extractant than the
other two.
The loading capacity of 0.03 M extractants was
studied from a feed solution containing 0.1 M Na2SO4
and varying the metal concentrations between 0.005
Fig. 1. Plot of equilibrium pH vs. log D. Org.: TOPS 99 (a); PC 88A and 0.04 M. Loading of the extractant with metal
(b); Cyanex 272 (c); Aq: 0.01 M Cd (II), 0.1 M Na2SO4. increases systematically with increase in metal con-
280 B. Ramachandra Reddy et al. / Hydrometallurgy 74 (2004) 277–283

centration and reaches maximum at z 0.02 M metal Table1

concentration. The corresponding percentage extrac- Effect of salts on percentage extraction of cadmium (II)
tion with respect to initial metal concentration S. no Extractant Salt Salt concentration (M)
decreases from 94% to 37% in case of TOPS 99 0.1 0.2 0.3 0.5 1.0
and from 98% to 36% in case of PC 88A and Cyanex Extraction of cadmium (%)
272. The loading capacity was calculated to be 1. TOPS-99 Na2SO4 71.0 70.7 69.6 67.2 63.0
1.62 F 0.05 g/L, which is equivalent to 99.1 –93.1% NaCl 83.8 83.6 81.0 73.0 66.0
of loading indicating that the extractants are almost NaNO3 75.2 75.0 74.8 73.9 73.4
pure in form. Further, the plot of log [Cd]Aq, M vs. log NaSCN 84.1 82.9 80.7 75.6 54.3
2. PC-88A Na2SO4 92.9 92.2 91.6 91.1 90.4
[Cd]Org, M for TOPS 99 (Fig. 3) is linear with a slope
NaCl 93.2 93.0 92.9 92.6 92.3
of f 0.7 indicating that monomeric metal species is NaNO3 92.5 91.7 91.0 90.1 89.3
extracted into the organic phase. Based on the results, NaSCN 95.3 93.4 91.5 90.0 88.9
the species extracted into the organic phase appears to 3. Cyanex-272 Na2SO4 99.97 99.96 99.95 99.95 99.95
be CdA2
5HA. NaCl 99.98 99.96 99.95 99.94 99.92
NaNO3 99.99 99.98 99.98 99.97 99.95
Extraction of Cd (II) from aqueous sulphate sol-
NaSCN 99.97 99.95 99.92 99.81 99.53
utions using the acid forms of TOPS 99, PC 88A and
Cyanex 272 in kerosene was poor. As a result, the
extractants were converted to sodium form (60%) by
the addition of sodium hydroxide. Considering the takes part in the extraction process of Cd (II) as given
results of Cd (II) extraction as a function of pH, by the equation:
extractant and metal obtained by slope analysis meth-
od, the mechanism can be proposed as follows: the  þ
Cd2þ
ðaqÞ þ AðorgÞ þ 3ðHAÞ2ðorgÞ ! CdA2 :5HAðorgÞ þ HðaqÞ
neutralization reaction of the extractants written as
(Sarangi et al., 1999; Reddy and Bhaskara Sarma, ð2Þ
2001):
Slope analysis from Figs. 1 and 2 supports the
Naþ þ
ðaqÞ þ 1=2ðHAÞ2ðorgÞ ! NaAðorgÞ þ HðaqÞ ð1Þ mechanism.

The acidic (Saji John et al., 1999; Ramachandra
Reddy et al., 2004) and neutral form of the extractant
Fig. 3. Plot of log metal (Aq) vs. log metal (Org). Org.: 0.03 M TOPS
99; Aq.: 0.1 M Na2SO4.
3.2. Effect of salts
The effect of salts such as Na2SO4, NaNO3, NaCl
and NaSCN (in the concentration range 0.1– 1 M) on
the extraction efficiency of 0.035 M TOPS 99, PC
88A and Cyanex 272 was studied for 0.01 M metal
(initial pH 2.85) The effect of salts on the percentage
extraction of metal by Cyanex 272 and PC 88A is
almost negligible. In case of TOPS 99 as extractant
and NaCl as salt, the percentage extraction decreases
from 83.6% to 66% whereas for NaSCN, the de-
crease is from 84.1% to 54.3%. The change in
equilibrium pH was 5.2 – 5.5 under the present ex-
perimental conditions. On the other hand, with
NaNO3, the percentage extraction changed margin-
ally from 75% to 73.4%. In case of Na2SO4, the
decrease was from 71% to 63%. The general con-
clusion is that Cd (II) extraction decreases with rise
in salt concentration when TOPS 99 is used as the
extractant (Table 1).
 B. Ramachandra Reddy et al. / Hydrometallurgy 74 (2004) 277–283 281

3.3. Stripping studies Table 3

Distribution coefficient values of Cd (II) using extractant (0.01M)
and synergist mixtures
The effect of acid concentration in the range 0.1–
DA, Extractant Concentration of DB Dmix SEF
1.0 M on the stripping of Cd (II) from 0.01 M LO
synergist (M)
(TOPS 99, PC 88A and Cyanex 272 in kerosene)
0.045(T) 0.005(P) Nil 0.385 8.6
containing 0.56 g/L Cd (II) was studied (Table 2).
0.045(T) 0.010(P) 0.01 0.722 14.4
More than 93% stripping efficiency of metal from 0.045(T) 0.015(P) 0.15 1.106 5.8
loaded organic phase was possible in one stage with 0.045(T) 0.020(P) 0.33 1.852 5.0
0.1 M HCl and H2SO4 and further increase in acid 0.045(T) 0.005(C) Nil 0.388 8.6
concentration showed marginal increase in efficiency. 0.045(T) 0.010(C) 0.01 1.486 26.5
0.045(T) 0.015(C) 0.06 1.874 17.8
On the other hand, in case of oxalic acid, two stages of
0.045(T) 0.020(C) 0.31 2.119 6.0
stripping was necessary to achieve >97% efficiency 0.005(P) 0.005(T) Nil 0.372 74.4
with acid concentrations z 0.5 M. 0.005(P) 0.010(T) 0.05 0.705 14.1
0.005(P) 0.015(T) 0.17 1.058 6.1
3.4. Synergism 0.005(P) 0.020(T) 0.41 1.915 4.6
0.005(P) 0.005(C) Nil 0.344 68.8
0.005(P) 0.010(C) 0.01 0.558 34.9
Blake et al. (1958) used the term ‘synergism’ to 0.005(P) 0.015(C) 0.06 1.257 19.3
describe the discovery of a definite enhancement of 0.005(P) 0.020(C) 0.31 1.866 5.9
extraction of uranium by mixture of an acidic alkyl 0.011(C) 0.005(T) Nil 0.338 30.7
phosphate and certain neutral organophosporous 0.011(C) 0.010(T) 0.05 0.638 11.4
0.011(C) 0.015(T) 0.17 1.113 6.2
esters, the resulting mixture giving a better extraction
0.011(C) 0.020(T) 0.41 1.948 4.6
of uranium than either the acid or the neutral phosphate 0.011(C) 0.005(P) Nil 0.328 29.8
alone. The effect is understood to be the replacement of 0.011(C) 0.010(P) 0.01 0.60 27.3
one extractant in the extracted complex by the other and 0.011(C) 0.015(P) 0.06 1.039 14.6
also due to various other factors. This property of the 0.011(C) 0.020(P) 0.31 1.746 5.4
mixed solvent system was utilised to study the extrac- T = TOPS 99; P = PC 88A; C = Cyanex 272.
tion behavior of cadmium using mixture of extractants DA = Distribution coefficient of cadmium with extractant.
DB = Distribution coefficient of cadmium with synergist.
(TOPS 99, PC 88A and Cyanex 272), keeping the Dmix = Distribution coefficient of the mixture.
concentration of one of the extractant constant at 0.01 SEF = Dmix/DA + DB
M and varying the other as synergist in the range of
0.005 – 0.02 M (Table 3). In case of TOPS 99 as
extractant, the synergistic enhancement factor (SEF) tration of synergist (PC 88A and Cyanex 272). On the
increased and then decreased with increase in concen- other hand, in case of PC 88A and Cyanex 272 as
extractants and others as synergist, SEF decreases with
Table 2 increase in synergist concentration. The results indicate
Effect of acid concentration on stripping of cadmium (II) from TOPS 99 as the best synergist.
loaded organic
S. no. Loaded organic [Acid] (M) Stripping (%) 3.5. Characterisation studies of Cd-TOPS 99 complex
HCl H2SO4 H2C2O4
1. TOPS-99 0.1 93.9 94.6 78.3 (92.9) 3.5.1. Infrared studies
0.5 94.3 96.9 89.6 (100) The Infrared spectra of TOPS-99 and Cd-TOPS 99
1.0 95.1 99.0 98.5 (100) solid complex indicate the absence of PU(OH) vibra-
2. PC-88A 0.1 96.0 97.7 81.4 (94.2) tion in the region 2750– 2550 cm 1, the absence of
0.5 98.2 98.8 84.1 (97.8)
1.0 98.3 99.4 89.4 (99.2)
PjO (OH) vibration in the region 2350 – 2080 cm 1,
3. Cyanex-272 0.1 96.2 95.5 46.0 (75.9) the absence of OUH deformation vibration at 1680
0.5 97.0 96.2 50.2 (98.6) cm 1, the shift of P – O bonded stretching vibration at
1.0 99.8 97.7 88.4 (100) 1225 to 1189 cm 1, the absence of PUOH bending
() = Two-stage stripping. vibration at 1115 cm 1, the absence of PjO (OH)
282 B. Ramachandra Reddy et al. / Hydrometallurgy 74 (2004) 277–283

vibration within 2700 –2550 cm 1 and the absence of

PUOU(H) antisymmetric stretching vibration at 1040
cm 1 (Peppard and Ferraro, 1959; Bellamy, 1975)
suggesting complex formation of Cd (II) by TOPS-99.

3.5.2. 31P NMR spectroscopy

Fig. 4 shows the 31P NMR spectra of TOPS 99 and
its Cd (II) complex. The 31P NMR of cadmium com-
plex showed a shift from 1.698 ppm (TOPS 99) to
3.016 ppm (Cd-TOPS 99 complex). A broad signal in
the 31P NMR spectra of the Cd-TOPS 99 complex was
observed although there was a small chemical shift
when compared with the extractant (TOPS 99). This

Fig. 5. Plot of equilibrium pH vs. percentage extraction of Cd and

Ni from their mixtures. Org.: 0.05 M TOPS 99 (a), PC 88A (b),
Cyanex27 (c); Aq.: 0.01 M Cd (5) and Ni (o), 0.1 M Na2SO4.

shift may be attributed to the coordination of cadmium

with UPO2 group of TOPS 99 (Lemire et al., 1985).

3.6. Extraction of Cd (II) and Ni (II) from mixture of

metals
Fig. 4. 31P NMR spectra of TOPS 99 (1) and Cd-TOPS 99 solid
complex (2). Org.: 0.2 M TOPS 99; Aq.: 0.1 M Cd (II), 0.1 M Studies have been carried out from sulphate sol-
Na2SO4. utions containing 0.01 M Cd (II) and Ni (II) using
 B. Ramachandra Reddy et al. / Hydrometallurgy 74 (2004) 277–283
0.05 M TOPS 99, PC 88A and Cyanex 272 dissolved
in kerosene (Fig. 5). The extraction of Cd (II) starts at
lower pH values than that of Ni (II) and increases
systematically with rise of pH with all the three
extractants. The observed pH0.5 (50% extraction)
values for Cd (II) and Ni (II) are 3.9 and 7.4 (DpH
(pH0.5 Cd –pH0.5 Ni) = 3.5) with TOPS 99, 5.9 and
7.35 (DpH = 1.45) with PC 88A and 4.2 and 7.5
(DpH = 3.3) with Cyanex 272, respectively, indicating
TOPS 99 to be an effective extractant for separation of
Cd (II) from Ni (II) considering better separation and
cost.
4. Conclusions
Solvent extraction studies of Cd (II) from sulphate
solutions by organophosphorus-based extractants es-
tablish the dependence of cadmium extraction on
equilibrium pH of the aqueous phase and extractant
concentration. The mechanism of metal transfer
involves 1:3 metal to extractant complex formation.
Addition of salts showed variable effect on percent
extraction of Cd (II). Mixtures of extractants indicated
TOPS 99 as the best synergist. The present results
demonstrate possible application to the separation of
Cd and Ni from the leach liquors of spent Ni –Cd
batteries/or any related materials.
Acknowledgements
The authors express their sincere thanks to
Ministry of Environment & Forests (MOEF), Gov-
ernment of India, New Delhi, India for the financial
support. Thanks are also due to Cytec Canada for
providing Cyanex-272 free sample.
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