Journal of EnvironmentalChemical Engineering1 (2013) 1269–1274

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Journal of Environmental Chemical Engineering

journal homepage: www.elsevier.com/locate/jece

Solvent extraction recovery and separation of cadmium and copper

from sulphate solution
Ehsan Bidaria,*, Mehdi Irannejada , Mahdi Gharabaghi
b

a
Department of Mining & MetallurgicalEngineering,Amirkabir Universityof Technology, Tehran, Iran
b
School of Mining Engineering,College of Engineering,Universityof Tehran,Iran

A RT I C L E I N F O ABST RACT

Article history: In this study solvent extraction process has been used for separation of cadmium and copper from
Received 12 July 2013 sulphatesolution.Aphosphoric acidextractant (D2EHPA)and anoxime extractant(MEX) inkerosene
Accepted 19 September 2013 diluent were used as cadmium and copper extractants, respectively. The results showed that 1g/L
cadmium could be extracted by 30–35% (v/v) D2EHPA at the pH of 3.5–4. Cadmium separation factor
Keywords: overcopperwithD2EHPAwascalculated4.04inbestconditionofpH(=2).Ontheotherhand3%MEX
Solvent extraction separated1g/LcopperovercadmiumoptimallyatthepHof3.5andunderthisconditionofpH,copper
Copper
separation factor is calculated 4495.5. Loading capacity studies showed that copper existence in
Cadmium
cadmium aqueous solution reduces cadmium extraction with D2EHPA up to 10% whilst copper
Phosphoric acid
Oxime extraction percentage with MEX does not vary considerably in the presence of cadmium.
2013 Elsevier Ltd. All rights reserved.

Introduction extracted from the by-products of zinc metallurgy among which

copper–cadmiumslag,cadmium–richdustandalsofromthespent
Eliminationofheavymetalsfromindustrialwastesatthepoint Ni-Cd batteries. Pure cadmium can be recovered through solvent
of environmental aspects was always important. Furthermore extraction, electrolysis refining or vacuum distillation [4].
there is an attitude toward the recovery of precious metals from Amongtheavailableprocessingalternatives,solventextraction
low-grade or complex ores, secondary resources and industrial is a technique that not only meets the strict environmental
wastes because of the reduction of world’s high grade resources regulations but also high purity value added products could be
and metals high prices. produced. Acidic extractants, including carboxylic acids, dialkyl
Generally, hydrometallurgical route (leaching–solvent extrac- phosphoric and dialkyl phosphinic acids, can be used to extract
tion–electrowinning)isfoundsuitabletoprocesslowergradeores, cadmium (II). The extraction of cadmium (II) is selective in the
wastes such as slag, tailings and recycled solutions [1]. Solvent presenceofZn(II),Ni(II),Co(II),Mn(II),Fe(II),Ca(II)andMg(II)with
extraction is now a very well-established process in hydrometal- DpH0.5(Me/Cd)=1.5 where Me=Zn (II), and not less than 2.5 for
lurgy. It is used for the hydrometallurgical processing of copper, the remainder of these cations. However, copper (II)and lead (II)
nickel, cobalt, zinc, uranium, molybdenum, tungsten, vanadium, canbeco-extracted[5].Differentkindsofextractantwereusedto
rare earths, zirconium, hafnium, niobium, tantalum, indium, extract cadmium from aqueous solution and a comprehensive
gallium,germanium,theplatinumgroupmetals,boron,reproces- literature about them are available [3,6].
sing nuclear fuels, purification of wet process phosphoric acid, Among phosphoric acids, (Di(2-ethylhexyl)) phosphoric acids
nitric acid recovery, etc. [2]. (D2EHPA) which is successfully used as cadmium extractant in
In this study recovery and separation of cadmium and copper severalindustrialandexperimentalworks,isusedinthisstudyand
were considered. Cadmium and its compounds are toxic and theextractionmechanismofthemetalion(inthiscasecadmium)
poisoning occurs through inhalation and ingestion. In spite of its with D2EHPA which is diluted in kerosene may be expressed as
toxicity, it is used in different industries such as electroplating, follows [7]:
pigments,syntheticchemicals,ceramics,metallurgicalandphoto-
nþ nþ p þ
graphicproducts,electronicsandotherindustries[3].Cadmiumis M þ ðH2A 2 Þorg @ ðMA n ðHAÞpÞorg þ nH (1)
2

where(H 2A 2)isextractantindimericform,Mismetal, n isvalence

* Correspondingauthor. Tel.: +98 914 8224306. ofthemetalormetalcomplexionand( n +p) numberofmolecules
E-mail address:
e.bidari@aut.ac.ir(E. Bidari). of extractant engaged in reaction. Working with concentrations

2213-3437/$– see frontmatter 2013ElsevierLtd. All rights reserved.

http://dx.doi.org/10.1016/j.jece.2013.09.016
1270 E. Bidari et al./Journal of EnvironmentalChemicalEngineering 1 (2013)1269–1274
[(Fig._2)TD$FIG]
lower than or equal to 0.2molL 1 (22.48g/L) of cadmium in the
organic phase, according to the literature [8], the chemical
reactions can be expressed as:

2þ þ
Cd þ 2ðH2A 2 Þorg @ CdA2 ðH2A 2Þorg þ 2H (2)

Inadditionofzincprocessingresiduescadmiumandcopperco-
existenceisseenindifferentmetalprocessingplants.Forinstance
thedensefumes,whichcomefromsmeltersofmetalbearingores,
are rich in metallic pollutants, such as Cd, Cu, Pb, and Zn [9].A
studywhichwasdoneinthevicinityofSarcheshmeh(thelargest
porphyrycopperdepositinIran)coppersmeltingplanshowedthat
SarcheshmehsoilsamplesareenrichedinAs,Cu,Mo,Zn,Cd,andPb
[10].Whereascoppersolventextractionisawell-establishedroute
in copper processing plants, copper extractants can also be
considered useful in the separation of cadmium and copper. The Fig. 2. Complexationof copperwith oxime extractants.
copper-specificextractantsusedtoextractcopperfromotherbase
metalsinacidicsulphateliquorsareknownas hydroxyoximes ,and
the interaction is known as chelation . The basic structures of
modernoximeextractantsareshowninFig.1andthecomplexa- ([HA]),whereasoptimumconditionofeachdesiredparameter(pH
tionofcopperbytheseextractantsisshownschematicallyinFig.2. or[HA])wasdeterminedbyvaryingthatparameterwhilstallother
Today modified aldoximes and aldoxime–ketoxime mixtures are parameters kept fixed. The condition at which highest extraction
themostwidelyusedcopperextractantsystems[11].Inthisstudy percentage happened, were chosen as optimum condition.
acadmiumcommonextractantcomparedwithacopperextractant Afterthat,asolutionofbothmetalswaspreparedandcontacted
atthepointoftheirabilityinselectiveseparationofcadmiumand withorganicphases(extractantwhichdilutedinkerosene).Metals
copperandalsoontheirloadingcapacitytowardeachandbothof concentrations in all aqueous phases were 1g/L. Equal volumes
these elements. (25mL)ofaqueousandorganicphasewereshakenusingincubator
shaker (stirring rate: 100rpm) for 20min in each test. Aqueous
Materials and methods solutionpHwasvariedfrom1to4.5andalltestswerecarriedin
room temperature.
Reagent After extraction process organic and aqueous phases were
separated using separatory funnel. The solutes (Cd or Cu), which
Theaqueousfeedsolutioncontainingcadmiumandcopperwas initiallywasdissolvedinaqueousphase(withinitialconcentration
preparedbydissolvingappropriateamountoftheirsulphatesaltin of [A0]aq) distributes between the two phases. Sample was taken
distilled water. Sulphuric acid (H 2SO 4) and sodium hydroxide fromaqueous phaseanditsmetal content([A1]aq )wasmeasured
(NaOH) solutions were used in order to maintain desired using Unicam 939 atomic absorption spectrophotometer. The
equilibrium pH of the solution during extraction. All chemicals flame conditions were those recommended by the instrument
used were analytical reagent grade. All inorganic reagents were manufacturer(wavelengths324.8nmand228.8nm,respectively,
purchased from Merck. ‘‘MEX’’ reagent from SOIL Company was forcopperandcadmium).Thequantificationlimitswere0.096mg/
used for solvent extraction of copper. This extractant based on L and 0.03mg/L and the detection limits were 0.29mg/L and
aldoxime and ketoxime molecules: 5-nonylsalicylaldoxime, 5- 0.01mg/L for copper and cadmium, respectively.
nonyl-2-hydroxyacetophenone oxime. Di-(2-ethylhexyl) phos- The distribution ratio of the solute can be calculated as
phoric acid (D2EHPA), from the Luoyang Zhongda Chemical Co. following:
Ltd. was of chemical reagent quality with a purity>95.0%, was
Aeq org
½ A0 aq ½ A1
½ aq
usedascadmiumextractant.Commercialgradekerosenewasused D¼ ¼
as diluent for organic extractant. Aeq aq
½ ½A1 aq

For practical purposes, as in industrial applications, it is often

Procedure
more popular to use the percentage extraction % E (sometimes
named the extraction factor), which is given by:
Experimental studies were carried in two steps. At first,
optimum condition of pH and extractant concentration for 100D
E
extracting of cadmium with D2EHPA and copper with MEX from % ¼ 1 þ D
theirpuresulphatesolutionofeachmetalweredetermined.Inthis
stage we have investigated the extraction process in order to
obtain optimum conditions of pH and extractants concentrations Results and discussion
[(Fig._1)TD$FIG]
Determination of optimum pH and extractant concentration

Acidic extractants include simple reagents such as carboxylic

Fig. 1. Modernoxime extractant.
acids and organophosphorus acids, as well as chelating acids,
extraction occurs by a change of the acidity in solution; thus,
increasing the pH of solution increases extraction. Acidic
extractants extract metals generally according to the following
equilibrium reaction:
zþ
M ðaqÞ þ zAHðorgÞ @ MA zðorgÞ þ zHþðaqÞ (3)
 E. Bidari et al./Journal of EnvironmentalChemical Engineering 1 (2013) 1269–1274 1271
Theextentofextractionalsodependsonthemagnitudeofthe [(Fig._4)TD$FIG]
metal–extractantformationconstantandconcentrationofextrac- 100
tant. These factors can be combined with the distribution 90
coefficient in the following equation derived from Eq. (1) and 80
Extraction%
the law of mass action [11]:
70
60
logD ¼logK f þ zlog½
HAþ zpH (4)
50
Cadmium
whereasD and Kf arethedistributioncoefficientofmetalandthe 40
equilibrium constant of reaction (3), respectively. Subsequently, 30
pH and extractant concentration have significant effect on metal 20
extractionandhavebeenreportedfrequentlyasmainparameters 10
in metals extraction and separation [6,12,13].
0
0 10 20 30 40
Optimum condition of cadmium extraction using D2EHPA
D2EHPA Concentration(v/v)%
EffectofpH.TheeffectofpHoncadmiumextractionfromsynthetic Fig. 4. Effect of D2EHPA concentration on cadmium extraction percentage; 1g/L
sulphate solution was examined in the range 0.5–4.5 at different cadmiumaqueoussolution;aqueousphasepH=3.5;O/Aphaseratio=1:1;shaking
D2EPHA concentrations. It was observed from Fig. 3 that the time=20min and in the room temperature.
percentage extraction depends mainly on the pH of the aqueous
phase. The extraction of cadmium starts at pH values around 0.5
and reaches quantitative extraction at initial aqueous phase pH Separation studies
3.5–4.0.
The selectivity of one metal over the other(s) is the ease of
EffectofD2EPHAconcentration. Aplotofcadmiumextractionusing isolating that metal from the mixed electrolyte solution and is
differentconcentrationsofD2EHPAispresentedinFig.4atinitial expressed in terms of the separation factor, SM1=M2 :
aqueous phase pH=3.5. It was observed that the D2EHPA
DM1
concentrationhadasignificanteffectonthecadmiumextraction. SM1=M2 ¼
Cadmium extraction increased by increasing D2EPHA concentra- DM2
tion up to optimum level whereas in which 1g/L cadmium where
extracted quantitatively by using 30–35% (v/v) D2EPHA.
nþ
M org
Dnþ ¼ nþ
Optimum condition of copper extraction using MEX M
M aq
nþ
Effect of pH.Initial experiments on the extraction of copper from
Dnþ
M is the distribution coefficient of the metal,M, between the
syntheticsulphatesolutionswereconductedintheinitialaqueous organicandaqueousphases.Thedistribution coefficient perseis
phasepHrange0.5–4.5usingdifferentconcentrationsofMEX.Asit notusefulinindustrialapplicationssinceitsvaluedependsonthe
is shown in Fig. 5 extraction was controlled by pH similar to operatingconditionssuchaspH,temperature,extractantconcen-
cadmium extraction and copper quantitatively extracted at tration, aqueous concentrations, phase ratio, etc. The separation
aqueous pH=3.5. factor, on the other hand, is a very useful variable in the
commercial applications, though its value also depends on the
Effect of MEX concentration.
Based on the previous results, the operating conditions. It is an indication of the ease of separating
effectoftheconcentrationofMEXontheextractionofcopperwas mixed electrolyte systems under a given set of operating
evaluatedatdistinctpHlevel(3.5),asshowninFig.6theincrease conditions. The higher the separation factor, the easier it is to
in the concentration of MEX resulted in higher metal extraction performselectiveextractionwithlittleornoco-extractionofother
whereas1g/Lcopperquantitativelyextractedusing3%(v/v)MEX. metals [14].

[(Fig._3)TD$FIG]
100 [(Fig._5)TD$FIG]
90 D2EHPA 5% 100
80 D2EHPA 15%
70 D2EHPA 25% 80 MEX 3%
Extraction%
60 MEX 1%
%
50 60
Extraction
40
30 40

20
10 20

0
0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 5 0
pH 0 1 2 3 4 5
pH
Fig. 3. Effect of pH on cadmium extraction percentage; 1g/L cadmium aqueous
solution; O/A phase ratio=1:1; shaking time=20min and in the room Fig.5. EffectofpHoncopperextractionpercentage;1g/Lcopperaqueoussolution;
temperature. O/A phase ratio=1:1; shaking time=20min and in the room temperature.
1272 E. Bidari et al./Journal of EnvironmentalChemicalEngineering 1 (2013)1269–1274
[(Fig._6)TD$FIG] [(Fig._7)TD$FIG]
100 1.1
1
90
0.9
80 0.8
Extraction% O/A=1:1
70 g/L 0.7
60 0.6
[Cd]org
0.5
50 0.4
3 1
Copper
40 0.3
30 0.2
0.1 2
20
0
10 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1 1.1 1.2 1.3 1.4
[Cd]aq g/L
0
0 1 2 3 4 5 6 Fig.7. Calculationofthenumberoftheoreticalstagesofextractionbythemethodof
MEX Concetration(v/v)% McCabe–Thiele(pH 3.5, [D2EHPA]=30% (v/v),O/A phase ratio=1:1).

Fig.6. EffectofMEXconcentrationon copperextractionpercentage;1g/Lcopper [(Fig._8)TD$FIG]

aqueous solution; aqueous phase pH=3.5; O/A phase ratio=1:1; shaking 90
time=20min and in the room temperature.
80
70
Cadmium separation over copper with D2EHPA
AnaqueousphaseofbothmetalswascontactedwithD2EHPA 60
Extraction%
(30%)indifferentpHconditions.Itwasconsideredthatmaximum 50
separation factor occurs at more acidic condition (pH=2) than
40
cadmiumoptimumextractionpH(ca.4).Theresultsareshownin Cu
Table 1. The pH 1/2 values calculated from 50% extraction of 30
Cd
cadmium and copper are 1.6 and 3, respectively, demonstrating 20
thepossiblequantitativeseparationofcadmiumandcopperfrom
10
their mixtures.
It is important to make a decision regarding the staging 0
requirements,asitisdirectlyrelatedtothecostofoperationand 0 5 10 15 20 25
maintenance.TheMcCabe–Thielediagramhelpstosetthenumber Time/min
ofextractionstagesneededinamixer-settlerfortheextractionof
Fig.8. Effectofcontacttimeoncadmiumandcopperextractionwith30%D2EHPA;
cadmium from the copper solution. Extraction isotherm was O/A phase ratio=1:1 and in the room temperature.
obtainedbycontactingthemetalssolutionand30%D2EHPA(v/v),
atdifferentA/Ophaseratiosfrom1to5andO/Afrom1to5atan
initial aqueous phase pH of 3.5. Fig. 7 indicates that 3 stages of Copper separation over cadmium with MEX
extractionwouldbesufficienttoextract100%cadmiumfromthe Samesolutionwithpreviousseparationtestwascontactedwith
solution having starting cadmium concentration of 1g/L at an MEX in order to study its capability in copper separation over
O=A ratio of 1.0. cadmium.Themetalssolutionwassubjectedtocopperextraction
Kinetic of cadmiumand copperextraction also wasstudied in insinglestageatdifferentinitialaqueousphasepHandA/Oratioof
which the effect of contact time on metals extraction has been 1:1 using 3% (v/v) MEX. Results which are shown in Table 2
considered using 30% (v/v) D2EHPA and pH=3.5. The results indicated that MEX is a very selective extractant for copper
obtained are shown in Fig. 8. The extraction of cadmium and whereas copper would be easily separated over cadmium in pH
copperwasrapidandattainedtheequilibriuminlessthan10min. rangeof2–4.5.Furthermore,optimumseparationpHoccursatthe
It was also observed that prolong contact time had no adverse same pH of maximum extraction percentage, so a quantitative
effect on extraction or separation. recovery and separation would be possible in pH around 3.5 in
Fig.9showstheeffectofstirringrateonmetalsextraction.Asit single stage.
isclearstirringratedonothaveaconsiderableeffectonextraction
percentageofcadmiumnorcopper.Thisindicatesthattheeffectof Loading capacity
the fluid to particle mass transfer resistance is negligible in both
cadmium and copper extraction with D2EHPA in stirring rates Loading capacity of D2EHPA and MEX were studied in the
higher than 50rpm. optimum conditions of pH and extractant concentration which

Table 1
Cadmium separationover copper with D2EHPA.

pH Distribution coefficientof cadmium Distributioncoefficient of copper Cadmium separationfactor over copper Cadmium extraction%

1 – 0.07 – 0
1.5 0.7 0.22 3.18 41.2
2 2.1 0.52 4.04 67.4
2.5 3.05 0.89 3.43 75.3
3 3.42 1 3.42 77.4
3.5 4.18 1.17 3.57 80.1
4 4.27 1.22 3.5 81.1
4.5 4.15 1.17 3.55 80.6
 E. Bidari et al./Journal of EnvironmentalChemical Engineering 1 (2013) 1269–1274 1273
[(Fig._9)TD$FIG] [(Fig._11)TD$FIG]
80 100
70
Cd
60 80
Extraction% Cu Extraction%
50

40 60

30
Copper
40
20

10
20
0
0 50 100 150 200
Stirring rate/rpm 0
0 1 2 3 4 5
Fig.9. Effectofstirringrateoncadmiumandcopperextractionwith30%D2EHPA;
pH
O/A phase ratio=1:1; shaking time=20min and in the room temperature.

[(Fig._10)TD$FIG] Fig. 11. Copper extraction with 30% D2EHPA; 0.1g/L copper aqueous solution;
differentpHofaqueousphase;O/Aphaseratio=1:1;shakingtime=20minandin
100 the room temperature.

90
[(Fig._12)TD$FIG]
80
100
70
n%
60
Extractio 90
50
Cd and Cu soluon
40 Extraction%
80
30
20 Cd soluon Cu soluon
70
10 Cu and Cd soluon
0
60
0 1 2 3 4 5
pH
50
Fig.10. Effectofcopperimpurityoncadmiumextractionpercentage;differentpH 0 1 2 3 4 5
of aqueous phase; O/A phase ratio=1:1; shaking time=20min and in the room
temperature.
pH

Fig.12. Effectofcadmiumimpurityoncopperextractionpercentagewith3%MEX;
differentpHofaqueousphase;O/Aphaseratio=1:1;shakingtime=20minandin
the room temperature.

were determined previously. It was found that cadmium extrac-

tion percentage increases with raising of D2EHPA concentration
(Fig.4)and30–35%D2EHPAcanextractcadmiumfromcadmium zinc hydrometallurgical plants whereas only removing of cadmi-
pure sulphate solution whilst copper existence in the solution um and copper from wastes, because of their environmental
reduces cadmium extraction percentage up to 10% (Fig. 10). problems, was important).
D2EHPA’s capacity for copper extraction was found approxi- It was also found that copper extraction efficiency increases
mately 10 times less than of its capacity toward cadmium with rising of MEX concentration (Fig. 6) and 2.5–3% MEX can
extraction and as Fig. 11 shows only 0.1g/L copper can extract extractcopperquantitativelyintheoptimumconditionofsolution
with 30% D2EHPA. Then D2EHPA can use for co-extraction of pH. Fig. 12 shows that cadmium existence in the solution has no
cadmium and copper whereas cadmium concentration in the noticeable effect on copper extraction, and then MEX is very
solution is several times more than copper concentration (e.g. insuitable solvent for separation of copper over cadmium.

Table 2
Copper separationover cadmiumwith MEX.
a
pH Distribution coefficientof copper Distributioncoefficient of cadmium Copper separationfactor over cadmium Copperextraction %

1 4.29 0 – 81.1
1.5 20.74 0.02 1037 95.4
2 51.63 0.02 2581.5 98.1
2.5 65.67 0.02 3283.5 98.5
3 82.33 0.02 4116.5 98.8
3.5 89.91 0.02 4495.5 98.9
4 82.33 0.02 4116.5 98.8
4.5 82.33 0.02 4116.5 98.8
a
Whereas all cadmiumdistribution coefficientswere in the range of 0.02
0.005, approximatedistribution coefficient (0.02) was taken to avoid the probable error.
1274 E. Bidari et al./Journal of EnvironmentalChemicalEngineering 1 (2013)1269–1274
Conclusion
OptimalcadmiumseparationovercopperwithD2EHPAoccurs
at more acidic and restricted pH than cadmium optimum
extraction pH, whilst MEX separated copper over cadmium with [5] L.Gotfryd,M.Cox,Theselectiverecoveryofcadmium(II)fromsulfatesolutionsby
grater separation factor and extended domain of pH. Loading
capacity studies revealed that 1g/L cadmium and 1g/L copper
could be extracted by using 30–35% D2EHPA and 2.5–3% MEX,
respectively. Then, whereas separation and recovery of these
elements was aimed, MEX is more effective extractant. Co-
extraction studies demonstrated that MEX has inconsiderable
extractioncapabilitytowardcadmiumwhilstD2EHPAcanextract
bothmetals,although,D2EHPA’scapacityforcopperisalmost10
times less than cadmium. So, whenever only removing of these [9] B.D. Tembo, K. Sichilongo, J. Cernak, Distribution of copper, lead, cadmium and
elements from wastes was concerned, D2EHPA can be more
suitable.
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