Hydrometallurgy 84 (2006) 155 – 164

www.elsevier.com/locate/hydromet

Kinetic mechanisms of cementation of cadmium ions by

zinc powder from sulphate solutions
S.R. Younesi, H. Alimadadi, E. Keshavarz Alamdari ⁎, S.P.H. Marashi
Department of Mining and Metallurgical Engineering, Amirkabir University of Technology, Hafez Ave, P.O. Box 15875-4413, Tehran, Iran
Received 15 February 2006; received in revised form 9 May 2006; accepted 22 May 2006
Available online 3 July 2006

Abstract

The cementation of cadmium ions by zinc powder was studied in a batch reactor at low and high concentrations at pH 5.2–5.4
and it is shown that the reaction is first-order. XRD and SEM analysis confirm that the deposited layer is metallic with no evidence
of basic zinc sulphate or re-dissolution of cadmium. Dependence of the reaction constant on initial cadmium concentration proves
the reaction mechanism. Different possible kinetic controlling models of cadmium ion (Cd2+) cementation from aqueous solution
by zinc powder were studied with respect to initial cadmium concentration, temperature, zinc powder size and stoichiometric ratio.
The experiments demonstrate that at initial cadmium concentrations > 1000 ppm, the ash diffusion control model prevails, while at
concentrations <500 ppm, the data has good agreement with the film diffusion model. For concentrations between 500 ppm and
1000 ppm, a combination of ash diffusion and film diffusion models controls the reaction rate. Based on numerical analysis, the
calculated activation energies at high and low concentrations are 9.6 and 7.2 kJ/mol, respectively. Statistical data analysis was
performed and different reaction rate constants were estimated from the equations for high and low initial cadmium concentrations.
© 2006 Elsevier B.V. All rights reserved.

Keywords: Cadmium cementation; Kinetics; Zinc powder; Mechanism

1. Introduction
The cementation process, which is known from an-
cient times, is considered as an important reaction in
hydrometallurgical processing and in winning metals.
Cementation is described as the electrochemical precip-
itation of a metal from solution by another more elec-
tropositive metal. Nowadays, cementation is one of the
most effective and economical techniques used in
hydrometallurgical zinc production for purification of
zinc sulphate solutions (Boyanov et al., 2004; Casaroli
⁎ Corresponding author. Fax: +98 21 6640 5846.
E-mail address: alamdari@cic.aut.ac.ir (E.K. Alamdari).
0304-386X/$ - see front matter © 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.hydromet.2006.05.005
et al., 2005) and for recovering toxic and precious metals
from industrial waste streams.
Cadmium is commonly found in zinc ores and is no-
bler than zinc. Thus, in the electrowinning process of
zinc, cadmium is deposited either before or simulta-
neously with zinc. This leads to the redissolution of zinc
in the acidic electrolyte and also acts as catalyst for
hydrogen evolution, which leads to a large drop in current
efficiency (Dobrev et al., 1998). As a result, cadmium
must be removed from the aqueous phase. Furthermore,
cadmium is considered as an extremely toxic heavy
metal, which is hazardous to the environment and espe-
cially to human health. Therefore, the prevention of
polluting natural water by cadmium ions is a very serious
issue in zinc production plants (Habashi, 1997).
156 S.R. Younesi et al. / Hydrometallurgy 84 (2006) 155–164
Cadmium ion (Cd2+) is usually removed from acidic
zinc sulphate solutions by cementation on zinc. The
electrochemical reaction can be described as:
Cd2þ þ ZnðsÞ →Zn2þ þ CdðsÞ ð1Þ
In previous publications, cementation reactions were
described by an overall first-order mechanism. Howev-
er, there still remains some uncertainty regarding the
cementation kinetics and reaction mechanism. Some
researchers have reported deviations from the first-order
kinetic plot (Guerra and Dreisinger, 1999; Hiskey and
Lee, 2003). Sêdzimir (2000) analyzed and commented
on the paper by Guerra and Dreisinger and basically
challenged the passivation model and the empirical rate
equation they had developed. Strong evidence of an
equilibrium model was presented to explain the negative
deviation from the first-order kinetic plot.
A phenomena commonly found in zinc dust cemen-
tation is the formation of basic zinc sulphate which slows
the process by forming a passivating layer on the zinc
dust surface (Singh, 1996; Nelson, 1998). The precip-
itation of basic zinc sulphate (BZS) during cobalt
cementation (Bøckman et al., 2000; Yang et al., 2006)
and lead cementation (Bear et al., 1995) by zinc was
observed. However, Ku et al. (2002) and Halikia and
Voudouris (2005) have reported that basic zinc sulphate
does not form during cadmium cementation by zinc.
Nevertheless, XRD analysis was performed to explore
the possibility of formation of basic zinc sulfate. Most
researchers have pronounced that the cementation of
cadmium ions by zinc is a first-order and diffusion con-
trolled reaction (Karavasteva, 1997; Ku et al., 2002;
Nosier, 2003; Taha and Abd El-Ghani, 2004).
Although cadmium ion removal by zinc powder is
thermodynamically very favorable (ΔG298° = −69.4 kJ,
equilibrium constant = 1.5 × 1012 at 25 °C (Lide, 1990), in
practice, equilibrium conditions are rarely approached.
The extent of reaction is determined by the reaction rate
rather than by the equilibrium thermodynamics. Conse-
quently, the information required for designing and oper-
ation purposes is associated with reaction rate rather than
ultimate equilibrium conditions. The importance of in-
creasing the reaction rate and decreasing zinc powder
consumption for industrial purposes have been considered
by several researchers, including Singh (1996). Reports
have been published on the effect of certain surfactants
(Karavasteva, 1997; Taha and Abd El-Ghani, 2004),
copper ions (Karavasteva, 1998) and ultrasound (Aur-
ousseau et al., 2004) to reduce process time. Although
several researchers considered the parameters that affect
the cadmium cementation rate system, i.e. temperature,
stirring speed, zinc particles size, amount of additives and
initial Cd2+ concentration in the solution; the kinetic
model of this process was not studied well. Halikia and
Voudouris (2005) studied the kinetics of the Cd2+/Zn
cementation system through a semi-theoretical approach
correlating the rates of zinc dissolution and cadmium
precipitation. Shen et al. (2003) studied some kinetic
models in an apparatus that resembles the continuous
industrial procedure. Finding the kinetic model of
cementation of Cd2+ by zinc will lead to better designs
on an industrial scale.
The aim of this work is to establish the kinetic model
of cadmium cementation by zinc powder, with respect to
batch industrial procedure, based on the models pre-
sented by Levenspiel (1999).
2. Experimental
2.1. Material
The cementation process was investigated by varying
the parameters affecting the reaction rate: i.e tempera-
ture, zinc powder size, initial cadmium concentration in
the solution, and the zinc powder stoichiometric ratio.
Zinc powder (purity > 99.5%, from Khorasan Powder
Metallurgy Inc.) was used as the sacrificing metal for
Cd2+ ions removal. Stock solutions of cadmium sulphate
(10 g/L) were prepared by dissolution of analytical grade
cadmium sulphate (Panreac) in double distilled water.
For each experiment, it was diluted to achieve the ap-
propriate cadmium concentrations (100–7500 ppm).
Zinc sulphate stock solution (60 g/L) was prepared by
dissolution of analytical grade zinc sulphate (Merck) in
double distilled water. It should be noted that the zinc ion
concentration in all solutions was 0.7 mol/L, which is
considered as the optimum zinc concentration in Iranian
zinc production plants.
2.2. Procedure
Reaction kinetic studies were performed with 200 ml
zinc sulphate, appropriate amount of cadmium sulphate
and double distilled water to maintain 250 ml solutions in
400 ml beakers set up in a constant temperature water
bath. A twin-bladed impeller, connected to a variable-
speed motor shaft, maintained an agitation rate of
600 rpm. The ratio of the impeller length to the diameter
of the beaker was 0.4, and the solution height to diameter
ratio of the beaker was 0.75. When the solution tem-
perature reached the desired value, the zinc powder was
added to the solution. This was marked as the beginning
of the experiment. The experiments duration was up to
15 min for all cases and 10 ml samples were withdrawn at
 S.R. Younesi et al. / Hydrometallurgy 84 (2006) 155–164
regular time intervals. Dissolved oxygen and pH were
measured by a METTLER MO128 and a METTLER MP
230, respectively. The samples were immediately vacuum
filtered using a 0.45 mm filter, then diluted and analyzed
for cadmium using atomic absorption spectrophotometry
(AAS). The cementation deposits were filtered, washed
with double-distilled water, dried and prepared for
scanning electron microscopy (Camscan MV2300).
Chemical composition of the cemented deposits was
determined by X-ray diffraction (XRD) using a Philips
Expert Pro with Cu cathode.
3. Results and discussion
3.1. XRD analysis
The formation of basic zinc sulphate (BZS), zinc oxide,
cadmium oxide, zinc hydroxide and cadmium hydroxide
during the cementation process is possible, which may
affect the reaction rate. According to TDS (total dis-
solved solid) diagrams presented by Halikia and Vou-
douris (2005) at ions concentration and pH of work, there
Fig. 1. X-ray diffraction analysis of solid particles from initial Cd = 1050 ppm.
157
is no precipitation of cadmium or zinc. To determine the
presence of these phases in the solid, experiments at ini-
tially 246 ppm and 1050 ppm cadmium concentration
were analysed. There was no significant difference in the
XRD of both deposits, which showed metallic cadmium
deposits on zinc surface with no indications of any alloy or
metal oxides/hydroxides on the surface (Fig. 1). However,
XRD analysis cannot reveal the phases with concentra-
tions lower than 5%.
3.2. pH and dissolved oxygen analysis
pH changes were measured during cadmium cementa-
tion with low (246 ppm) and high (1050 ppm) initial cad-
mium concentration. When the starting pH was 5.2–5.4,
the pH increased to 5.8–6.1 within 1 min, due to re-dis-
solution of zinc oxide on the surface oxidized zinc powder,
and then remained almost constant. Little alternation of pH
during cadmium cementation showed that re-dissolution of
cadmium did not occur.
Another phenomenon that can occur during cemen-
tation is re-oxidation due to the presence of dissolved
158 S.R. Younesi et al. / Hydrometallurgy 84 (2006) 155–164

Fig. 2. SEM backscatter micrograph of the surfaces of zinc powders (a)

before cementation, (b) after 5 min cementation at initial Cd = 246 ppm
(c) after 10 min cementation at initial Cd = 1050 ppm.

oxygen. Experiments conducted at low (246 ppm) and

high (1050 ppm) initial cadmium concentration found that
the dissolved oxygen value before starting was 2.2–
2.3 mg/L and decreased to 1.6–1.9 mg/L upon adding Fig. 3. SEM photograph of deposited layer on zinc powder at initial
zinc powder. It then remained constant during cementa- Cd = 1050 ppm.
tion indicating re-oxidation of cadmium does not occur.
(a). Secondary electron image.
As the amount of deposited cadmium is very low at the
(b). X-ray map image of cadmium.
beginning, the small decrease in DO is attributed to re- (c). X-ray map image of zinc.
action with excess zinc powder, which also leads to pH
increase.

Zn þ O2 þ 2H2 O→Zn2þ þ 4OH þ 2e ð2Þ

 S.R. Younesi et al. / Hydrometallurgy 84 (2006) 155–164 159

3.3. Morphology study 3.5. Effect of initial cadmium concentration

SEM was used for a morphological study of cemented The effect of initial cadmium concentration on frac-
deposits at low and high initial cadmium concentrations. tional cementation vs. time was investigated at constant
The morphology of the unreacted zinc powder is pre-
sented in Fig. 2a, while typical examples of the deposited
cadmium morphology are shown in Fig. 2b and c.
Comparing these figures it can be concluded that the
morphology of powder remains more or less spherical,
and that the deposited layer after 10 min (Fig. 2c) is
denser than the layer formed after 5 min (Fig. 2b). Ini-
tially, cadmium nucleation and growth takes place at low
angular, high energy sites and then extends to other parts.
The presence of cadmium lamellar plates on zinc powder
can easily be seen after 5 min (Fig. 2b). However, as the
reaction progresses and zinc particles are covered by
cadmium, the growth of these plates continues, producing
a dense structure (Fig. 2c).
To examine the layers density, zinc granules with 2–
3 mm diameter were added to the solutions containing
1050 ppm cadmium, allowed to react for 15 min, and
then mounted and analyzed by SEM. The results, shown
in Fig. 3, illustrate the build up of a thick cadmium metal
layer onto zinc with little zinc within the dense cadmium
layer. Similar results were obtained with the 246 ppm
cadmium solution, although the layer was thinner and
less dense indicative of the lower cementation rate.
The results confirm that and shrinking core model
prevails. To determine the kinetic controlling model, the
shrinking core models, suggested by Levenspiel (1999),
were utilized. The studied models are described in detail
in the Appendix.

3.4. Reaction order

One of the best methods to study reaction order is the

Integral Method in which the curve of − ln(C / C0) vs.
time would be considered for investigations of first-
order reactions. Fig. 4a-c show the variations for
different initial cadmium concentrations. The slopes of
− ln(C / C0) vs. time for all concentrations < 500 ppm are
approximately linear up to 1000 s (Fig. 4a). However, in
concentrations > 1000 ppm the reaction is first-order
only during first 300 s (Fig. 4b) and there is a noticeable
deviation from first-order at very high cadmium
concentration (Fig. 4c).
The slope of −ln(C / C0) vs. time indicates the reaction
constant. In elementary reactions the reaction constant is
independent of reactants concentrations. However, as can
Fig. 4. Effect of initial cadmium concentration on variation of first-
be seen in Fig. 4a and b, there is an obvious dependence of order plots. (20 °C, zinc powder size −170 + 325#, stoichiometric ratio
reaction constant on initial cadmium concentration. To find Zn : Cd = 5:1) a) initial Cd < 500 ppm, b) initial Cd > 1000 ppm, c)
the reaction mechanism, further studies were performed. deviation at extended times.
160 S.R. Younesi et al. / Hydrometallurgy 84 (2006) 155–164

3.6. Effect of temperature

As the concentration analysis could not indicate a

unique mechanism, the activation energy of the reaction
and the effect of zinc powder size were investigated in
order to specify the kinetic controlling model. Activation
energy of chemically controlled reactions is > 40 kJ/mol;
while diffusion controlled reactions have activation
energies of about 10 kJ/mol or less (Levenspiel, 1999).
To calculate the activation energy, experiments con-
ducted at different temperatures at constant initial con-
centration (1050 ppm or 246 ppm) under the same
conditions as above. Fig. 6a and b plot ln K′ vs. 1 / T at
high and low concentration for all three studied models.
Based on the slope analysis, the calculated activation
energies for ash diffusion are 5.8 and 12.6 kJ/mol at low
and high concentrations, while the calculated activation
energies for film diffusion are 10.3 and 22.1 kJ/mol
respectively. All these values are in the expected range of
diffusion controlled reactions, except for 22.1 kJ/mol.
The calculated activation energies for the chemical
reaction model at low and high concentrations are 7.3
and 13.4 kJ/mol, respectively. Therefore, it can be con-
cluded that the chemical reaction could definitely not be
the kinetic controlling mechanism.

3.7. Effect of zinc powder size

The effect of zinc powder size was studied to verify

Fig. 5. Effect of initial Cd concentration on fractional cementation vs.
time. (conditions as Fig. 4.) a) initial Cd > 1000 ppm, b) initial
Cd < 500 ppm.
the mechanism since Eq. (a-3) and Eq. (a-6) of Appendix
indicate that the slopes of ln K′ vs. ln r for film diffusion
and ash layer control are − 1 and − 2, respectively. The

Table 1
temperature (20 °C), stoichiometric ratio of zinc pow- Reaction rate constants and their linear correlation residual values for
shrinking core model at various initial cadmium concentrations
der to cadmium in solution (5:1) and zinc powder size
(− 170 + 325#) over the initial cadmium concentration Chemical Ash diffusion Film diffusion Concentration
reaction control control for control for (ppm)
range from 109 ppm to 7250 ppm to study the kinetics for spherical spherical spherical
and mechanism at both low and high concentrations. particles particles particles
The results, shown in Fig. 5a and b, were examined
R2 K′ × 103 R2 K′ × 103 R2 K′ × 103
under different controlling models and are compared in (s− 1) (s− 1) (s− 1)
Table 1. The data presented in this Table suggests that
0.99 0.06 0.92 0.01 0.99 0.18 109
at initial cadmium concentration < 500 ppm, film 0.99 0.12 0.90 0.03 0.99 0.34 184
diffusion and chemical reaction controlling models 0.98 0.15 0.80 0.04 0.99 0.39 205
for spherical particles prevail; while at concentrations 0.99 0.16 0.87 0.05 0.99 0.43 246
> 1000 ppm, ash diffusion and chemical reaction 0.99 0.24 0.94 0.12 0.97 0.67 395
0.99 0.29 0.93 0.16 0.99 0.77 474
control models for spherical particles give higher cor-
0.58 0.87 0.83 0.51 0.38 2.06 864
relation results. The data for cadmium concentrations 0.95 0.81 0.99 0.40 0.91 2.01 1050
between 500 ppm and 1000 ppm shows no accuracy 0.96 1.21 0.99 0.98 0.89 2.69 2010
with any of the mentioned models. It can be concluded 0.96 1.49 1.00 1.21 0.88 3.08 2720
that reaction kinetic mechanism is changing in the 0.93 2.33 1.00 2.13 0.75 4.39 4800
0.93 2.67 1.00 2.81 0.55 4.15 7250
range of 500–1000 ppm.
 S.R. Younesi et al. / Hydrometallurgy 84 (2006) 155–164 161

Fig. 7. Variation of ln K′ vs. ln d.

Fig. 8 for 246 ppm cadmium concentration. The observed

decrease in the fraction of cadmium cemented with
decrease in the stoichiometric ratio could be attributed to:
(i) less effective surface area of zinc (ii) increasing mean
thickness of deposited cadmium layers, which results in
mass transfer decrease. The kinetic model tends to be film
diffusion controlled by increasing the stoichiometric ratio
to near 10:1. In this case, a narrow cadmium layer covers
the surface of zinc particles, through which the cadmium
ions easily penetrate and mass transfer of cadmium ions
in the liquid phase controls the reaction rate.

3.9. Experimental equation for estimating reaction rate

Fig. 6. Variation of ln K′ vs. inverse temperature. (other conditions as
Fig. 4) a) initial Cd = 1050 ppm, b) initial Cd = 246 ppm. constant

Initial cadmium concentration, temperature and zinc

results of experiments conducted with different zinc grain size data, were statistically analyzed by SPSS V8
powder sizes under the same conditions (Fig. 7) shows software using a multi-variable linear model. For initial
that the slope of ln K′ vs. ln d curve, (where d = mean
diameter zinc powder), is −1 for cadmium concentra-
tions <500 ppm; and − 2 for concentrations > 1000 ppm.
It is worth mentioning that decreasing zinc powder size
at high concentrations has more effect on cadmium
removal than at low concentrations.
The combination of initial cadmium concentration,
temperature and zinc powder size studies proves that at
high concentrations of cadmium (> 1000 ppm), ash
diffusion controls the reaction rate, and at low concen-
trations (< 500 ppm), film diffusion is the kinetic
controlling model.

3.8. Effect of stoichiometric ratio on kinetic model

Fig. 8. Fractional cementation vs. time for different stoichiometric ratio
The stoichiometric ratio was studied as another of Zn : Cd in solution at initial Cd = 246 ppm. (other conditions as
effective parameter on rate of reaction, as shown in Fig. 4).
162 S.R. Younesi et al. / Hydrometallurgy 84 (2006) 155–164
Fig. 9. Deviation of experimental values of ln K′ from adjusted
predicted values derived from equation for low initial cadmium
concentrations.
cadmium concentrations > 1000 ppm where ash diffu-
sion is the kinetic controlling model, the reaction rate
constant equation is described by:
ln K V¼ 2:39 þ 1:03ln Cd;0  2:02ln r
1159:7
 R2 ¼ 0:99
T
and for initial cadmium concentrations < 500 ppm, the
equation is:
ln K V¼ 4:71 þ 0:94 ln CCd;0  1:10 ln r
861:3
 R2 ¼ 0:98
T
The deviation of experimental values of ln K′ from
adjusted values predicted by the equations is demon-
strated in Fig. 9.
In Section 3.6, the effects of temperature and
activation energy were calculated without considering
data obtained on varying zinc powder size. Simultaneous
analysis of all experimental data by linear multi-variable
method of SPSS software provided more accurate
activation energy at high and low initial concentrations
of cadmium of 9.6 and 7.2 kJ/mol, respectively.
4. Conclusions
XRD analysis reveals that basic zinc sulphate does
not form during the cadmium cementation on zinc and
the deposited layer was entirely metallic. Little alterna-
tion of pH and dissolved oxygen during the process
indicate that re-dissolution and re-oxidation of cadmium
does not occur. SEM analysis show that the deposited
layer is dense and the shrinking core model prevails. Based
on experimental results, it is shown that the cementation of
cadmium ions by zinc powder is a first-order reaction at
initial cadmium concentrations <500 ppm and is film
diffusion controlled with a calculated activation energy of
7.2 kJ/mol. At concentrations >100 ppm there is consi-
derable deviation from first-order after 300 s and ash dif-
fusion is the proper kinetic controlling model with a
calculated activation energy of 9.6 kJ/mol. Between
500 ppm and 1000 ppm, the kinetic model is a com-
bination of film diffusion and ash diffusion control. De-
creasing the zinc powder size at high concentrations is
more effective than at low concentrations. A high stoi-
chiometric ratio about 10:1 is required to maintain film
diffusion control. By decreasing the stoichiometric ratio,
the kinetic model tends to be ash diffusion controlled. The
overall adjusted equation for prediction of ln K′ for high
concentration is:
1159:7
ln K V¼ 2:39 þ 1:03ln Cd;0  2:02ln r 
T
and for low concentrations is:
ð3Þ 861:3
ln K V¼ 4:71 þ 0:94 ln CCd;0  1:10 ln r 
T
Nomenclature
b Stoichiometric factor
CCd2+ Cadmium concentration
CCd2+,0 Initial cadmium concentration
ð4Þ K′ Reaction rate constant (min− 1)
Kl Mass transfer coefficient between liquid and
particle
K″ First-order rate coefficient for the surface reaction
K0 First order rate constant for the surface reaction
De Effective diffusion coefficient of liquid reac-
tant in the ash layer
D0 Diffusion coefficient constant
Q Activation energy (kJ/mol)
rC Radius of unreacted zinc
r Initial zinc radius
t Time
R Universal gas constant
T Recorded temperature (K)
XCd Cadmium fractional conversion
ρZn Zinc density
δ Film layer thickness over zinc particle
Acknowledgement
The authors would like to thank Mr. S. Dehghan for
his help in performing some of the experiments.
 S.R. Younesi et al. / Hydrometallurgy 84 (2006) 155–164 163

Appendix A or:
 
V 6bD0 Q
For the non-catalytic reactions of particles with ln KADC ¼ ln þ ln ðCCd Þ  2lnðrÞ 
surrounding fluid, a shrinking core model was consid- qZn RT
ered. In this model it is visualized that reaction occurs ða  6Þ
first at the outer skin of the particles. The reaction zone
then moves into the solid, leaving behind completely Chemical reaction control for spherical particles:
converted material and inert solid. Three different steps Using the mass balance technique for chemical
can be recognized in shrinking core reactions such as reaction conditions:
cadmium cementation by zinc particles in which no gas 1

or liquid is produced. These steps are described below. 1  ð1  XB Þ3 ¼ K Vt ða  7Þ

This determines the kinetic controlling model of

Step 1 Diffusion of Cd2+ through the film surrounding reaction, where:
the zinc particles to the surface of the solid.


Step 2 Penetration and diffusion of Cd2+ through the V bKWCCd bK0 exp  RT CCd
Q

blanket of ash to the surface of the unreacted KCRC ¼ ¼  ða  8Þ

qZn r qZn r
core.
Step 3 Reaction of Cd2+ with zinc particles at this or:
reaction surface.
V bK0 Q
ln KCRC ¼ ln  þ lnCCd  lnr ða  9Þ
Each of these steps could control the reaction rate. qZn RT
Therefore, three different models could be the reaction
mechanism with their constant rate equations mentioned
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