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Study on the extraction of palladium(II)

and platinum(IV) using LIX 84I
Article in Hydrometallurgy October 2006
DOI: 10.1016/j.hydromet.2006.04.005

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Hydrometallurgy 84 (2006) 54 59
www.elsevier.com/locate/hydromet

Study on the extraction of palladium(II) and

platinum(IV) using LIX 84I
M.V. Rane a,, V. Venugopal b
a

Hydrometallurgy Section, Materials Group, BARC, Trombay, Mumbai-400 085, India

Radiopharmaceutical and Isotope Group, BARC, Trombay, Mumbai-400 085, India

Received 28 February 2006; received in revised form 21 April 2006; accepted 25 April 2006
Available online 19 June 2006

Abstract
The extraction behaviour of Pd(II) and Pt(IV) was studied with LIX84 I (2-hydroxy-5-nonylacetophenone oxime) in HCl
medium. The distribution ratios of Pd(II) with LIX 84I are sufficiently high to extract Pd(II) from 0.1 M HCl medium. The Pd-LIX
84I complex has been identified with slope and saturation loading methods. Some thermodynamic values like G, H and S for
the Pd-LIX 84I have been determined. The extraction of Pt(IV) with LIX 84I was poor from hydrochloric solutions. However, Pt
(IV) was extracted from ammoniacal solutions. The back extraction of Pd(II) was carried out using 6 M HCl and Pt(IV) using 1 M
SnCl2 in 3 M HCl. Pd(II) and Pt(IV) were separated from common impurities like Fe(III), Al(III), Zn(II), Cu(II) and Ni(II) using
LIX 84I. The recoveries of palladium and platinum were 97% and 86%, respectively.
2006 Elsevier B.V. All rights reserved.
Keywords: Palladium; Platinum; LIX 84I; Solvent extraction

1. Introduction
Solvent extraction is one of the methods for the
separation and purification of Pd(II) and Pt(IV) from
acidic solutions. One of the commercial applications
was the extraction of Pd(II) using di-(n-octyl) sulphide
(DOS) in Esso Isopar M (Edwards, 1979). Pd(II) has
also been extracted with hydroxyoxime extractants
(Cleare et al., 1979, 1981; Ma and Freiser, 1983; Hoh
et al., 1984; Inoue and Maruuchi, 1986) and alkylated
derivatives of 8-hydroxyquinoline like Kelex 100 and
LIX 26 (Demopoulos, 1986).

Corresponding author. Fax: +91 22 25505151.

E-mail address: r_v_mahesh@rediffmail.com (M.V. Rane).
0304-386X/$ - see front matter 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.hydromet.2006.04.005

The separation of Pt(IV) from Pd(II) in the presence

of stannous chloride have been cited. Pd(II) was
extracted from 0.75 to 2.0 M HClHClO4 acid mixtures
using PC-88A in toluene (Bandekar and Dhadke, 1998).
Pd(II) and Pt(IV) have been separated from iron(III),
cobalt(II), nickel(II) and copper(II) in hydrochloric acid
medium using N-n-octylaniline in xylene (Lokhande et
al., 1998a,b). The extraction of Pd(II) has been reported
with various extractants, viz. tris-iso-octylamine (Mirza,
1980), triphenylphosphine (Mojski, 1980), tri-n-octylamine (Hasegawa et al., 1991), cyanex 471 (Hidaigo et
al., 1991), diamine extractants (Shillington and Tait,
1991), cyanex 301 (Takahiko et al., 1994) and LIX 63
(Foulon et al., 1999a,b).
The present paper describes the extraction and back
extraction of Pd(II) and Pt(IV) using LIX 84I (Cognis,
Mining chemicals technology; Website: http://www.

M.V. Rane, V. Venugopal / Hydrometallurgy 84 (2006) 5459

cognis-us.com/). The effect of various parameters like

feed pH, extractant concentration, chloride concentration, etc. on the distribution ratios of the Pd-LIX 84I
system has been studied. The composition of Pd-LIX
complex was elucidated using slope method and
saturation loading. Thermodynamic data was generated
for the Pd-LIX system. Pd(II) was separated from Pt(IV)
and impurities using LIX 84I.
2. Experimental
A stock (5 g/l) solution of Pd(II) in 1 M HCl was
prepared by dissolving the pure metal powder (99%) in
aquaregia. The solution was evaporated several times
with conc. HCl and the residue was dissolved in 0.1 M
HCl. A stock solution of Pt(IV) was prepared by
dissolving sodium salt of hexa-chloroplatinic acid in
dilute HCl to obtain a solution containing approximately
1 g metal/l. Palladium was estimated as Pd-DMG
complex by gravimetry. Pt(IV) was first precipitated as
ammonium chloroplatinate, ignited and estimated as
metal. Feed solutions of the desired concentration were
prepared from these stock solutions.
Palladium and platinum (above 0.1 g/l) were determined by atomic absorption spectrometry (ModelGBC Avanta, Australia). Below 0.1 g/l, platinum was
determined by UV visible spectrophotometry (ModelGBC Cintra, Australia) using stannous chloride method
(Ayres and Meyer, 1951). The active component (2hydroxy-5-nonylacetophenone oxime) in the solvent
was determined by potentiometric titration of the
protons liberated during extraction of Cu2+ (Preston,
1975).
2.1. Extraction of Pd(II) and Pt(IV) using LIX 84I
For determining the distribution ratio, organic and
the aqueous phases were contacted for the stipulated
time. The phases were separated. The metal ion
concentration in aqueous phase was determined after
filtering through Whatman No. 42 to remove any traces
of the organic material. Wherever, the organic phase was
required to be analyzed, it was first filtered through 1PS
Whatman to remove the entrained aqueous phase. The
distribution ratios, D = [M]org/[M]aq were calculated
from the aqueous metal ion concentration before and
after equilibrium. [M]org and [M]aq are the metal ion
concentrations in the organic and aqueous phases,
respectively. Back extraction was studied using different
reagents like HCl, HNO3, SnCl2 and H2SO4.
For regeneration of the extractant, the used organic
phase was contacted with equal volume of DM water for

55

15 min. The phases were separated and the pH of the

aqueous phase was measured. The organic phase was
given repeated contacts with fresh DM water until there
was no change in pH. The organic phase was then
reused.
2.2. Separation of Pd(II) and Pt(IV) from impurities
Synthetic solutions containing 0.25 g/l Pt(IV) and
varying concentrations of Pd(II) were used for determining the separation factors.
For the separation of Pd(II) and Pt(IV) from common
impurities, a synthetic feed containing 1 g/l each Pd(II),
Pt(IV), Fe(III), Al(III), Zn(II), Cu(II) and Ni(II) was
prepared. 250 ml of the synthetic feed solution was
taken and its pH was adjusted to 2.0. It was contacted
with 250 ml of 0.15 M LIX 84I in dodecane for 2 h to
extract Pd(II). The two phases were separated. The
loaded organic phase was labeled as organic 1 and the
aqueous phase as aqueous 1. The impurities were
scrubbed from organic 1 three times with 50 ml each of
1.5 M H2SO4. The aqueous phase from the three
contacts was collected together as strip 1. Then, Pd(II)
was stripped three times with 50 ml each of 6 M HCl.
The aqueous phase from these three contacts was
collected together as strip 2. The pH of aqueous 1 was
adjusted to 9.0 by addition of liquor ammonia. The
solution was filtered through Whatman No. 42. The
residue was discarded. The filtrate was contacted with
equal volume of 0.15 M LIX 84I in dodecane for 30 min
to extract Pt(IV). The two phases were separated as
organic 2 and aqueous 2. The impurities were scrubbed
from organic 2 three times with 50 ml each of 1.5 M
H2SO4. The aqueous phase from the three contacts was
collected together as strip 3. Then, Pt(IV) was stripped
three times with 50 ml each of 1 M SnCl2 in 3.5 M HCl.
The aqueous phase from these three contacts was
collected together as strip 4. For scrubbing and
stripping, a contact time of 1520 min was provided.
3. Results and discussion
All distribution ratios were measured in triplicates
and the mean value was taken. The agreement of the
values is within 5%.
3.1. Extraction of Pd(II) using LIX 84I
The % extraction of Pd(II) with LIX 84I was
measured at different time interval at a pH of 1.0. The
data is given in Fig. 1. From this data, it was observed
that the extraction was more or less constant after

56

M.V. Rane, V. Venugopal / Hydrometallurgy 84 (2006) 5459

Fig. 2. Plot of log D versus feed pH.

Fig. 1. Determination of equilibrium time for extraction of Pd(II) with
LIX 84I.

60 min. Hence, in all subsequent experiments, for the

determination of distribution ratios, an equilibration
time of at least 60 min was maintained.
The effect of feed pH on the extraction of Pd(II)
with LIX 84I in dodecane was studied. LIX 84I is
capable of extracting Pd(II) in pH range. The %
extraction is given in Table 1. It is evident that
extraction increases with pH, attains a maximum value
at pH 3.0 and decreases thereafter. The H + ion
concentration at equilibrium (i.e. equilibrium pH)
depends on two factors; the initial feed pH and the
H+ ions liberated during the extraction process. At
lower feed pH, the contribution from the H+ ions
liberated during the extraction is insignificant. Hence,
the equilibrium pH depends on the feed pH and the
extraction increases with feed pH. At higher feed pH,
the equilibrium pH is essentially governed by the H+
ions liberated during extraction. Hence, the extraction
is almost constant (96% extraction) in the pH range
2.03.0. However, when the feed pH is adjusted to 4,
the precipitation of palladium commences.

It was observed that at pH 23, the % extraction is

high. It is seen from the data that the distribution ratios
are high enough to quantitatively extract Pd(II) in a
single contact. The plot of D versus pH was found to be
a straight line with slope of approximately 2 (Fig. 2).
Distribution ratios of Pd(II) were measured by
varying the chloride concentration. It can be observed
from the data that when the chloride concentration is
increased, the distribution ratio decreases. The increase
in the chloride concentration favours the formation of
PdCl42 complex. As a result, the concentration of free
Pd(II) ion decreases. Therefore, the distribution ratio
decreases with increase in chloride concentration. The
plot of log D versus log[Cl](aq) was found to be a
straight line with negative slope of approximately 4
(Fig. 3).
The D values for Pd(II) with LIX 84I are enhanced
with the increase in the extractant concentration. A plot
of log D versus log[HL] was drawn and found to be a
straight line with slope near to 2 (Fig. 4). This implied

Table 1
Effect of feed pH on % extraction of Pd(II) with LIX 84I
Sr. no.

Feed pH

Equilibrium pH

% Extraction

1
2
3
4
5

1.0
1.5
2.0
3.0
4.0

1.0
1.5
1.9
2.4
2.7

30
65
94
97
72a

Organic = 0.015 M LIX 84I in dodecane, aqueous = 0.15 g/l Pd,

equilibration time = 60 min, agitation = 300 rpm.
a
The precipitated palladium collects at the interface of the two
phases.

Fig. 3. Plot of log D versus log[Cl].

M.V. Rane, V. Venugopal / Hydrometallurgy 84 (2006) 5459

Fig. 4. Plot of log D versus log[HL].

57

Fig. 5. Plot of ln Keq versus 1/T.

that the extractant combined with Pd(II) in the ratio

of 2:1.
Based on the above studies, the following extraction
mechanism has been proposed:

PdCl2
4 2HLPdL2 4Cl 2H

The above mechanism was compared with the results

obtained for saturation loading of 0.015 M LIX 84I. As
per the proposed mechanism, 0.015 M LIX 84I should
load 0.0075 M of Pd(II), which corresponds to
0.795 g/l of Pd. The fully loaded organic was found
to contain 0.8 g/l of palladium, which agreed with the
theoretical value. This further confirmed that palladium forms a complex with the extractant in 1:2 ratio.
The extraction behavior of LIX 84I with Pd(II) was
studied with different diluents at a fixed feed pH of 2.0.
The diluents studied were aliphatic as well as aromatic.
Diluents like dodecane, benzene, toluene and xylene
were used. The results are given in Table 2. It can be
observed from this data that the extraction of Pd(II) with
LIX 84I is more or less same with all diluents except
dodecane. However, when dodecane was used, the
extraction improved significantly. This was found to be
true at pH 1.0 and 1.5 also. In general, the order of
extraction was benzene < toluene < xylene < dodecane.

This illustrated that the extraction improved with

increasing number of aliphatic branches in the aromatic
diluents.
The values of H and S, in the temperature
range of 3050 C, were calculated from the plot of
ln Keq versus 1/T (Fig. 5). The values obtained were
155 kJ/mol and 532 J/mol/K, respectively. The positive
value of H denotes that the extraction process is
endothermic. The positive entropy and the slightly
negative G suggest that the reaction proceeds in the
forward direction (Table 3).
For back extraction studies, feed containing
1.9 g/l palladium (pH = 1.5) was contacted with
0.075 M LIX 84I. The loaded LIX 84I was back
extracted with different reagents. It was observed that
back extraction is not possible even with 2 M H2SO4.
HNO3 reacted with the extractant. Back extraction was
also tried with 2 M, 4 M and 6 M HCl. Quantitative back
extraction could not be achieved with 2 M and 4 M HCl.
Only 60% of the loaded Pd(II) was back extracted.
However, complete back extraction was observed with
6 M HCl in two contacts. It was observed that more than
90% of the loaded Pd(II) was back extracted in a single
contact. A contact time of 10 min was found to be
Table 3
Thermodynamic data for the Pd-LIX 84I system

Table 2
Effect of diluents on the extraction of Pd(II) with LIX 84I
Sr.
no.

Feed
pH

Distribution ratio, D
Benzene

Toluene

Xylene

Dodecane

1
2
3

1.0
1.5
2.0

0.12
0.18
0.29

0.18
0.23
0.34

0.22
0.36
0.46

0.43
1.8
16

Organic = 0.015 M LIX 84I in dodecane, aqueous = 0.15 g/l Pd,

A/O = 1.

Temperature (C)

Distribution ratio, D

Keq

G (kJ/mol)

30
35
40
45
50

0.67
1.1
1.6
2.4
3.3

12.0
32.6
85.0
218
539

6.33
9.00
11.6
14.3
17.0

Organic = 0.015 M LIX 84I in dodecane, aqueous = 0.80 g/l Pd

(pH = 1.5), equilibration time = 23 h, agitation = 300 rpm.

58

M.V. Rane, V. Venugopal / Hydrometallurgy 84 (2006) 5459

Table 4
% Extraction in each extractionstrippingregeneration cycles

Pd extracted (g/l)
% Extraction

Table 6
Separation of Pd(II) and Pt(IV) using 0.015 M LIX 84I

Cycle
1

Cycle
2

Cycle
3

Cycle
4

Cycle
5

Cycle
6

1.04
54.74

1.02
53.68

1.05
55.26

1.03
54.21

1.03
54.21

1.01
53.16

sufficient to attain the equilibrium. Degradation of the

extractant was observed at higher concentrations of HCl
(> 6 M).
After back extraction of metal from the organic
phase, the extractant was regenerated. As hydrochloric
acid was used for back extraction, the entrained acid
raises the equilibrium pH in the subsequent cycle. This
decreases the % extraction in the next cycle. Before
recycling the extractant, the stripped organic solvent
was, therefore, washed with DM water to remove the
entrained acid. It was observed that the extraction
behavior of this used organic solvent for Pd is same as
earlier.
After studying the regeneration, the extractant was
subjected to six cycles of extractionstrippingregeneration. The % extraction was determined at the end of
each cycle. The data is given in Table 4. The %
extraction was more or less constant in all cycles. It was
observed from this data that the extractant was stable to
the reagents employed and this was further confirmed
by determining the loading capacity of the extractant for
copper at the end of the sixth cycle. It was found to be
4.99 g/l (theoretical loading = 4.81 g/l Cu).
3.2. Extraction of Pt(IV) using LIX 84I
It was observed that Pt(IV) was not extracted by LIX
84I below pH 8.0 (Table 5). Above pH 8.0, the
extraction of Pt(IV) by LIX 84I was possible in
ammoniacal medium and it increased with increasing
pH. However, the precipitation of Pt(IV) as ammonium
chloroplatinate beyond pH 9.0 interfered with the
extraction process. In view of these difficulties, it was
not possible to study the system.
Table 5
Effect of feed pH on the extraction of Pt(IV) by LIX 84I
Feed pH

1.0

2.0

3.0

4.0

7.0

8.0

9.0

Pt(aq) (g/l)
Pt(org) (g/l)
Distribution
ratio, D

0.97
<0.01
<0.01

0.97
<0.01
<0.01

0.97
<0.01
<0.01

0.97
<0.01
<0.01

0.97
<0.01
<0.01

0.90
0.07
0.08

0.38
0.59
1.5

Organic = 0.015 M LIX 84I in dodecane, aqueous = 0.97 g/l Pt,

equilibration time = 60 min, agitation = 300 rpm.

Sr.
no.

1
2
3
4
5

Feed conc. (g/l)

Distribution
ratio, D

Separation factor
= DPd(II)/DPt(IV)

Pd(II)

Pt(IV)

Pd(II)

Pt(IV)

0.20
0.30
0.40
0.60
0.80

0.25
0.25
0.25
0.25
0.25

16
12
8.3
4.1
2.4

0.04
0.04
0.04
0.04
0.04

400
300
208
102
60

The back extraction of Pt(IV) from the loaded

organic was attempted using HCl and H2SO4 of varying
concentrations up to 6 M and 2 M, respectively. These
reagents were found to be unsuitable for back extraction.
Due to the higher stability of the Pt(IV)-LIX 84I
complex, the back extraction of Pt(IV) from the loaded
organic is difficult. It was found that quantitative back
extraction (> 98%) was achieved with a reducing
stripping agent like 1 M SnCl2 in 3 M HCl in three
contacts.
3.3. Separation of Pd(II) and Pt(IV) using LIX 84I
The results of the single contact experiments using
mixed synthetic solutions of Pd(II) and Pt(IV) are given
in Table 6. Since Pt(IV) is not extracted by LIX 84I from
acidic medium, Pd(II) can be easily separated from Pt
(IV). Pd(II) is extracted into the organic phase, while Pt
(IV) remains in the aqueous phase.
Experiments were also carried out using synthetic
solution to separate Pd(II) and Pt(IV) from other
impurities. The synthetic feed contained 1 g/l each Pd
(II), Pt(IV), Fe(III), Al(III), Zn(II), Cu(II) and Ni(II).
The feed solution was equilibrated with 0.15 M LIX 84I
in dodecane to extract Pd(II). The feed pH was adjusted
to 2.0. As a result, the equilibrium pH stabilized at 1.5,
which prevented the extraction of Fe(III) [extraction of
Fe(III) commences beyond 1.5 pH]. However, at this
pH, Cu(II) was also extracted along with Pd(II). From
this loaded organic, Cu(II) was selectively scrubbed
with 1.5 M H2SO4. Then, Pd(II) was back extracted with
6 M HCl.
Table 7
Separation of Pd(II) and Pt(IV) from impurities
Stream Pd(II)

Pt(IV) Cu(II)

Strip 1 <0.005 ND
Strip 2 1.61 ND
Strip 3 <0.005 ND
Strip 4 <0.005 1.43

Ni(II)

Zn(II)

Fe(III)

Al(III)

1.45 <0.005 <0.005 0.010 ND

0.020 <0.005 <0.005 0.007 ND
<0.005 1.52
0.30 <0.005 0.009
<0.005 0.007 0.016 <0.005 ND

All concentrations in g/l. ND: not detectable.

M.V. Rane, V. Venugopal / Hydrometallurgy 84 (2006) 5459

For Pt(IV) extraction, the pH of aqueous1 was

adjusted to 9.0 by addition of liquor ammonia. Fe(III)
and Al(III) were precipitated. The Pt(IV) in the filtrate
was extracted alongwith Ni(II) and Zn(II) using LIX
84I. From the loaded organic, Ni(II) and Zn(II) were
selectively back extracted with 1.5 M H2SO4. Then, Pt
(IV) was back extracted with 1 M SnCl2 in 3 M HCl.
The analysis data of the different strip solutions is
shown in Table 7.
4. Conclusion
LIX 84I extracts Pd(II) in the pH range of 1 to 3. It
forms a Pd-LIX complex in the stoichiometric ratio of
1:2. Back extraction of Pd(II) is achieved using 6 M
hydrochloric acid. Pt(IV) is extracted by LIX 84I
beyond pH 7.0 and is back extracted with 3 M HCl
containing stannous chloride. Pd(II) and Pt(IV) have
been separated from common impurities like Fe(III), Al
(III), Zn(II), Cu(II) and Ni(II) using LIX 84I. Thus, LIX
84I has been used for the separation as well as the
purification of Pd(II) and Pt(IV).
Acknowledgement
One of the authors is thankful to Dr. A.K. Suri,
Associate Director (P), Materials Group, and Shri S.K.
Tangri, Head Hydrometallurgy Section for permitting
him to undertake the work.
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