696 J. Mater. Sci. Technol., Vol.22 No.

5, 2006

Kinetics of Silver Dissolution in Nitric Acid from Ag-Au0.04 -Cu0.10

and Ag-Cu0.23 Scraps
S.K.Sadrnezhaad† , E.Ahmadi and M.Mozammel
Center of Excellence for Advanced Processes of Production of Materials, Department of Materials Science
and Engineering, Sharif University of Technology, Tehran, Iran
[Manuscript received September 27, 2005, in revised form January 30, 2006]

Kinetics of dissolution of silver present in precious metal scraps in HNO3 was studied in temperature range of
26∼85◦ C. Dissolution rate of silver was much faster than that of copper at all temperatures. Effects of particle
size, stirring speed, acid concentration and temperature on the rate of dissolving of silver were evaluated.
Dissolution rate decreases with particle size and increases with temperature. Dissolving was accelerated with
acid concentrations less than 10 mol/L. Concentrations greater than 10 mol/L resulted in slowing down of the
dissolution rate. Shrinking core model with internal diffusion equation t/τ =1−3(1−x)2/3 +2(1−x) could be
used to explain the mechanism of the reaction. Silver extraction resulted in activation energies of 33.95 kJ/mol
for Ag-Au0.04 -Cu0.10 and 68.87 kJ/mol for Ag-Cu0.23 particles. Inter-diffusion of silver and nitrate ions through
the porous region of the insoluble alloying layer was the main resistance to the dissolving process. Results
were tangible for applications in recycling of the material from electronic silver-bearing scraps, dental alloys,
jewelry, silverware and anodic slime precious metal recovery.
KEY WORDS: Silver; Copper; Kinetics, Dissolution; Shrinking core model; Internal diffusion

1. Introduction tics of pyrolusite of Mn-Ag ores in presence of hy-

Silver is used as an alloying element, coating mate-
rial, ornament, catalyst and biosensor[1,2] in medicine,
battery and film industry[2,3] . Silver nitrate has a
wide application in electroplating, painting, xerogra-
phy and chemical processing. Silver is produced di-
rectly from its ores or as a by-product of zinc, cop-
per and lead[3∼5] . The world consumption of silver
exceeds its mine production rate. Silver containing
articles must, therefore, be recycled in order to partly
cover its consumption[6] . Recovery of the scrapped
products plays an important role in fulfillment of the
increasing silver demand in a foreseeable future.
A common process used in precious metals in-
dustry to separate silver from gold is nitric acid
dissolution[7∼12] . Alloys with high silver content can
be directly treated with HNO3 to dissolve their sil-
ver content and to leave the undissolved elements as
a separable solid phase[12] . This method is prefer-
ably used in small-scale processes like alloy refinement
when aqua regia dissolution is not a suitable treat-
ment.
Many investigations on silver/copper reaction
with nitric acid solutions can be found in litera-
ture [7∼10]. Schack and Clemmons[11] illustrated a
high temperature treatment of silver scrap via smelt-
ing and cupellation. Martinez et al.[12] report on sil-
ver molar fraction that substantially affect on the rate
of silver nitrate formation. With both high nitric acid
activity and temperature, Martinez et al.[12] showed
an outward diffusion of nitrate molecules within the
undissolved gold containing less than 0.65 mol frac-
tion of silver[12] to control the dissolution rate. At 0.7
and more silver mole fraction, a solid-surface chemi-
cal mechanism with activation energy of 54.3 kJ/mol
prevails. Jiang et al.[13] illustrated the leaching kine-
† Prof., Ph.D., to whom correspondence should be addressed,
E-mail: sadrnezh@sharif.edu; sadrnezh@yahoo.com.
drogen peroxide. The activation energy obtained by
them is 4.45±0.3 kJ/mol at 30∼60◦ C in nitrate[13] .
Traditional recovery of precious metals from anode
slime consists of fusion of sludge in presence of flux,
cupellation, melting with-lead in a cupel and parting.
Lead is oxidized by atmospheric oxygen and absorbed
by the magnesite in the cupel. This leaves gold, sil-
ver and platinum group elements as a button, which
can be weighed to determine the total content of the
precious metals. This usually contains too much gold
to be separated by nitric acid treatment.
Kunda[14] applied an alternative hydrometallurgi-
cal silver extraction method, which consisted of (a)
sulfuric acid leaching of the silver bearing materials,
(b) dilution in water of the product, (c) dissolving
in dilute ammonia of the precipitate and (d) reduc-
tion with hydrogen of the precipitate into silver[14] .
Similar processes can be applied to the solid waste
materials containing silver bearing substances. Ultra-
sound can help to increase the rate of the leaching
process[15] .
The precious metals such as gold, silver, selenium
and tellurium can be recovered from the anodic slim
by (a) nitric acid leaching, (b) liquid-liquid extraction
and (c) direct reduction[16,17] . In comparison with
the conventional pyrometallurgical processes, Wang
et al.[16] claimed hydrometallurgical process to be eco-
nomic, energy-saving and pollution-free.
Demir et al.[18] determined a semi-empirical ki-
netic model for dissolution of metallic copper parti-
cles in HNO3 . Their results showed 18.81 kJ/mol
of activation energy. Kinetics of reaction be-
tween metallic silver and nitric acid was investi-
gated by Ozmetin et al.[19] in the concentration range
of 7.22∼14.44 mol/L. Their results have shown a
surface reaction control with activation energy of
57.66 kJ/mol.
Literature lacks essential information on kinetics
 J. Mater. Sci. Technol., Vol.22 No.5, 2006 697
of silver recovery from silver bearing waste materials
such as electronic wastes, photographic films, spent
catalysts and jewelry scraps. Significant amounts of
these materials are created these days throughout the
world[20,21] . This paper aims to elucidate the kinet-
ics and mechanism of dissolution of silver present in
Ag-Au0.04 -Cu0.10 and Ag-Cu0.23 scraps in nitric acid.
The results are useable to improve recovery of pre-
cious metals from silver bearing scraps and wastes[22] .
It is therefore of value to the newly growing materials
recycling technologies[20∼22] .
Fig.1 Effect of acid concentration on fractional dissolu-
2. Experimental tion of silver of Ag-Au0.04 -Cu0.10 alloy

Ag-Cu0.23 ingots were produced by melting and

casting of analytical grade raw materials in alumina
crucibles. Chemical composition of the samples is
85 wt pct Ag and 15 wt pct Cu. Pieces of metals (sil-
ver and copper) were weighted, charged and heated up
to 1050◦ C for 15 min. Alloy filings were made of the
ingot by hack sawing of the specimens. The empirical
data obtained by Rubcuminintara and Tasaso[6] for
Ag-Au0.04 -Cu0.10 jewelry scraps having 86.91 wt pct
Ag and 5.89 wt pct Cu were also used for data veri-
fication and comparison purposes. The experimental
conditions used in this research are similar to those.
Dissolving experiments were carried out in a one-
liter cylindrical container immersed into a thermostat-
ically controlled water bath. Test temperatures were
selected in the range of 26 to 85◦ C. After the container
was warmed up to the required temperature, it was
fed with 250 ml of aqueous HNO3 being stirred with
a specified rate. The stirring rate remained constant
during each test and one gram of filings was added to
the container. At selected time intervals, 5 ml solu-
tion was sampled. The samples were diluted to the
desired volume in a volumetric flask. The analysis of
the diluted samples was made with an atomic absorp-
tion spectrophotometer (AAS).
Dissolution kinetics was determined by analyzing
the dissolved silver. Assuming that there exists a
spontaneous reaction, fractional extraction can be de-
fined as the ratio of the concentration of the metal-
lic species present in the solution at time t divided
by its total amount in the alloy. The apparatus was
calibrated with a series of well known standard solu-
tions. The uncertainties of the measurements were es-
timated with regression analysis procedure. The cor-
relation coefficient (R2 ) was found to be in the range
of 0.98∼0.99.
3. Results and Discussion
Different mixing speeds were used to monitor the
effect of stirring on the rate of dissolution of the sil-
ver. The rate of dissolution did not change with the
speed of mixing. This finding was consistent with the
data reported by previous authors[6] . Therefore, ex-
ternal transfer was not the controlling step for silver
dissolution.
Other influential parameters were concentration,
alloy particle size and temperature. Figure 1 shows
the effect of nitric acid concentration on fractional dis-
solution of silver. It can be seen from Fig.1 that the
dissolution rate increases with acid concentrations up
to ∼10 mol/L HNO3 and then decreases beyond this
Fig.2 Effect of particle size on fractional extraction of
silver and copper at 26◦ C. Part of the data is ob-
tained from literature [6]
concentration. A maximum is therefore observable at
∼10 mol/L nitric acid concentration.
Martinez and Espiel[12] investigated the effect of
nitric acid concentration on dissolution rate of sil-
ver in Ag-Au alloys and found that the reaction was
first order with 51.1 and 75.12 pct silver at 80◦ C and
3.8∼7.10 mol/L nitric acid concentrations. For alloys
with 51.1 pct silver and acid concentrations exceeding
6 mol/L, the reaction order dropped to zero. HNO3
reduced generally to NO2 at these concentrations.
For leaching silver from copper anode slime, it was
reported that there is an optimum nitric acid concen-
tration of about 7 mol/L[23] . This value was lower
than the acid concentrations corresponding to the
maximum rate of extraction of silver in this investiga-
tion. According to Butts and Coxe[24] , the solubility
of silver nitrate in water decreases considerably with
the nitric acid concentration. The decrease in dis-
solution rate of the silver beyond ∼10 mol/L HNO3
concentration seems therefore to be due to this ef-
fect. The concentration for dissolution experiments
was chosen 10.4 mol/L.
Effect of particle size on fractional extraction of
silver in the nitric acid solution is depicted in Fig.2.
As is seen, the dissolution rate decreases with aver-
age size of the particles. The silver dissolution rate
seems, therefore, to be sensitive to the internal (pore)
mass diffusion step. This contradicts with the conclu-
sion mentioned by previous researchers, who claimed
a single-step chemical control mechanism[6] .
Figure 3 shows that the amount of copper extrac-
tion is much less than that of silver, especially at low
temperatures. However, both rates increase dramat-
ically with temperature. A much faster dissolution
process was therefore observed at 85◦ C than at room
temperature. A comparison of the extraction data for
Ag-Cu0.23 and Ag-Au0.04 -Cu0.10 alloys given in Fig.4
698 J. Mater. Sci. Technol., Vol.22 No.5, 2006

reactions[6,12] .
3Ag(s)+4HNO3 (aq) → 3AgNO3 (l)+NO(g)+2H2 O(l)
(1)
Ag(s) + 2HNO3 (aq) → AgNO3 (l) + NO2 (g) + H2 O(l)
(2)
With alloy compositions and nitric acid concentra-
tions used in this investigation, Reactions (1) and (2)
are spontaneous at room temperature. Sum of the
two reactions is as follows:
4Ag(s) + 6HNO3 (aq) → 4AgNO3 (l) +
NO(g) + NO2 (g) + 3H2 O(l) (3)
At high nitric acid concentrations, the following reac-
tions may also become feasible[7∼9] :
2Cu(s)+4HNO3 (aq) → Cu(NO3 )2 (aq)+
Cu(NO2 )2 (aq) + 2H2 O(l) (4)
Cu(NO2 )2 (aq) + 2HNO3 (aq) →
Fig.3 Effect of temperature on extraction: (a) silver and Cu(NO3 )2 (aq) + 2HNO2 (aq) (5)
(b) copper from Ag-Cu0.23 alloy having a particle
size of 75∼150 µm with 10.4 mol/L HNO3 and a Cu(s) + HNO3 (aq) + HNO2 (aq) →
stirring rate of 250 r/min Cu(NO2 )2 (aq) + H2 O(l) (6)
Cu(NO2 )2 (aq) + 2HNO3 (aq) →
Cu(NO3 )2 (aq) + 2HNO2 (aq) (7)
HNO2 (aq) + HNO3 (aq) → 2NO2 (g) + H2 O(l) (8)
Cu(s)+4HNO3 (aq) → Cu(NO3 )2 (aq)+
2NO2 (g) + 2H2 O(l) (9)
Dissolution reaction of silver depends on the ni-
tric acid concentration. With a dilute acid, Eq.(1)
is applicable. With a concentrated one, Eq.(2) pro-
ceeds further. For simplicity, we chose Eq.(3), which
Fig.4 Effect of temperature on fractional extraction of is a combination of two reactions. With nitric acid,
silver from Ag-Cu0.23 and Ag-Au0.04 -Cu0.10 alloys HNO2 has a catalytic effect on dissolution of copper.
leached with 10.4 mol/L HNO3 at 250 r/min. The Nitrogen dioxide can react with water to form nitric
data on ternary alloys are from literature [6] acid (compare Eqs.(8) and (9)). We have, therefore,
chosen Eq.(9) for our evaluations.
The standard Gibbs free energy change (∆G◦ ) in
Table 1 Thermodynamic properties of substances at Reactions (1)∼(9) can be determined from ∆Hf◦ and
298 K and 105 Pa[27] S ◦ data of compounds and elements (see Table 1).
Substance ∆Hf◦ /(kJ/mol) S ◦ /(J/mol·K)
Standard Gibbs free energies in Reactions (3) and (9)
Ag(s) 0 42.68
are, thus, obtained to be −209.06 and −196.20 kJ/mol
Cu(s) 0 33.14 at 298 K and 105 Pa, respectively. If all activities are
AgNO3 (l) −124.52 140.92 considered unity, the reactions seem spontaneous at
Cu(NO3 )2 (aq) −350 193 room conditions. Figure 3 shows that Reaction (3) is
HNO2 (aq) −119 46.1 more favorable than Reaction (9) under the experi-
HNO3 (aq) −207 53.5 mental conditions used in this research. Therefore, it
H2 O(l) −286 69.95 is logically reasonable to assume the activity of silver
NO(g) 90.2 211 greater than that of copper and gold.
NO2 (g) 33.2 240 Reactions (1)∼(3) require NO− 3 /Ag
+
ion trans-
port between the reaction-site and the bulk-liquid
indicates that the presence of gold in the scrap has phase. The experimental data obtained in this re-
an increasing effect on the rate of extraction of sil- search were used to check the different kinetic mod-
ver especially at lower temperatures. This implies a els available for solid-fluid reactions[26] . Since copper
positive interaction parameter of gold on silver in Ag- and gold do not favor reaction with HNO3 at room
Au0.04 -Cu0.10 alloys employed in this study[25] . temperature, a porous metallic layer composed of Cu
The closest kinetic mechanism indicates the op- (and Au) remains on the surface of the un-reacted Ag-
timal condition for maximum recovery of silver from Cu0.23 (or Ag-Au0.04 -Cu0.10 ) core. The radius of the
silver containing metallic objects. From thermody- scrap grains does not, therefore, considerably change
namics, the spontaneity of the dissolution process can with advancement of the reaction.
be predicted. The dissolution reaction of the impure Pore diffusion control with constant particle-size
alloys in nitric acid can be expressed by several typical gave the best answer with correlation coefficients
 J. Mater. Sci. Technol., Vol.22 No.5, 2006 699
greater than 0.96. For spherical particles having the
average initial radius of R0 , the total conversion time
τ is defined by the following equation.

ρa R02
τ= (10)
6bDe cA

where ρa is the molar density of the alloy; b is the stoi-

chiometric coefficient of the reaction (3/4, 1/2 and 2/3
for Eqs.(1), (2) and (3), respectively); De is the coeffi-
cient of inter-diffusion of Ag+ and NO− 3 ions through
the porous metallic layer and cA is the concentration
of HNO3 in the bulk solution. Reactant and product
ions, i.e. NO− 3 and Ag
+
ions, must diffuse through-
out the pores in order to obtain an on-going reaction.
De is the inter-diffusion coefficient of NO− 3 and Ag
+

indicating ion transfer within the porous region.

The reaction between silver and nitric acid is of
electrochemical nature. Because of considerable con-
ductivity of the metallic layer, there is no resistance
to charge transfer through the solid region. The only
remaining resistance is thus related to the NO− 3 and
Fig.5 Internal diffusion plot for silver dissolution:
Ag+ ion transfer through the aqueous electrolyte that (a) Ag-Cu0.23 alloy at different temperatures and
fills the porous region of the solid phase. This resis- (b) Ag-Au0.04 -Cu0.10 particles at different acid
concentrations
tance is considered by the inter-diffusion coefficient
De in the present system.
The dimensionless conversion time relevant to the
pore diffusion mechanism can be obtained by the fol-
lowing equation:

t
= 1 − 3(1 − x)2/3 + 2(1 − x) (11)
τ
Silver dissolution plot on the right side of Eq.(11) is
depicted against time in Fig.5. Regression analyses
of the data indicated correlation values of 0.99 at dif-
ferent temperatures. Other model correlations were Fig.6 Effect of initial radius on the total extraction time
plotted against time. No cases gave better straight of silver from Ag-Au0.04 -Cu0.10 alloy
lines than those in Fig.5.
The data plotted in Fig.2 confirms the above con- tortuosity are two important factors that affect the
clusion. As it is seen, the size of the alloy particles amount of the diffusion coefficient in porous regions.
has a substantial effect on the extraction rate of the De = D(Ag+ /NO− ) εθ (12)
silver. In order to assess the quantitative relationship 3

between the total conversion time and the average
size of the particles, the slopes of the curves shown in
Fig.5 were plotted vs R0−2 , as shown in Fig.6. The
straight line regression equation was found to have a
correlation factor of 0.98. It was, therefore, assessed
once more that the silver dissolution from the alloys
into the nitric acid was controlled by diffusion.
The effective internal diffusion coefficient De was
estimated from Eq.(10). The density of the Ag-
Au0.04 -Cu0.10 scrap is nearly 11.03 g/cm3 while that
of Ag-Cu0.23 is about 10.25 g/cm3 (estimated from
densities of pure elements with an ideal solution
model). The average initial size of the filings was used
from the sieve analyses data. The results obtained
was De =7.59×10−7 cm2 /s for Ag-Au0.04 -Cu0.10 and
5.76×10−7 cm2 /s for Ag-Cu0.23 scrap at room tem-
perature.
The radius of Ag+ ions (0.113 nm) is smaller than
that of Ag atoms (0.144 nm). On the contrary, the
radius of NO− 3 ions (0.200 nm) is larger. Consider-
ing geometry of the system, it may be concluded that
the pore diffusion for Ag+ /NO− 3 ions is not easy for
their transfer within the bulk phase. Porosity and
where DAg+ /NO− is bulk inter-diffusion coefficient; ε
3
is porosity and θ is the tortuosity coefficient of the
porous region.
Bulk diffusion coefficient of AgNO3 in aqueous
HNO3 media is reported to be 1.71×10−5 cm2 /s at
room temperature[28] . The inter-diffusion coefficients
obtained in this research are mush smaller than this.
Considerable difference between these coefficients in-
dicates significant influence of the electrochemical and
geometrical characteristics of the present porous sys-
tem.
AgNO3 has lower solubility at higher acid con-
centrations (cHNO3 ≥10 mol/L). Solid precipitate
may thus partially block the reaction front at
cHNO3 ≥10 mol/L. Rate controlling mechanism can
hence locally change from pore diffusion into transfer
in solid phase. The reaction rate is therefore reduced
due to lowering of De inside the porous layer.
The frequency factor and the activation energy of
dissolution of silver are thus determined using the Ar-
rhenius law.
De = D0 e−Q/RT (13)
700 J. Mater. Sci. Technol., Vol.22 No.5, 2006
Table 2 Activation energies and frequency factors
evaluated from application of the silver dis-
solution data to the mathematical model
developed for internal transfer of silver into
nitric acid solution
Alloy Q/(kJ/mol) D0 /(cm2 /s)
Ag-Au0.04 -Cu0.10 33.95 0.73
Ag-Cu0.23 68.87 2.27×106
where D0 is the frequency factor and Q is the acti-
vation energy of the diffusion. R is the universal gas
constant and T is the absolute temperature of the so-
lution. The results is illustrated in Table 2. The val-
ues evaluated for the activation energies of the silver
supported the porous metallic layer diffusion. Con-
siderable reduction in frequency factor of silver due to
presence of gold in the alloy implies the significant in-
teraction between the two species of the system. This
could be the matter of further investigation.
4. Conclusions
(1) Based on the data presented in this paper, the
rate of reaction with nitric acid of the silver contained
in jewelry scrap, silver-copper and silver-copper-gold
alloys are influenced by particle size, acid concen-
tration and temperature. Insertion of the empirical
data into different solid-fluid kinetic models indicated
a shrinking core internal diffusion equation explain-
ing the mechanism of the reaction. The kinetic data
showed a linear relation of 1−3(1−x)2/3 +2(1−x) with
time. The apparent activation energies obtained de-
pend on the chemical species present in the scrap
phase.
(2) An effective inter-diffusion coefficient, De ,
of 7.59×10−7 cm2 /s for Ag-Au0.04 -Cu0.10 and
5.76×10−7 cm2 /s for Ag-Cu0.23 scrap was obtained
for ion transfer through the porous silver-less layer
formed at exterior of the particles because of disso-
lution of silver at room temperature. The maximum
rate of dissolution occurs between 7.9 and 10.4 mol/L
acid concentration. This is due to lower water solu-
bility for AgNO3 in presence of nitric acid at 26◦ C.
Previous investigators have recognized the Ag-
Au0.04 -Cu0.10 grains size effects on the rate of silver
dissolution[6] . This finding is also backed-up by our
further measurements (Fig.2). The extraction rate
decreases, for example, by increasing of the size of
the particles dissolving in the nitric acid solution as
shown in Fig.2. This result is in obvious contradic-
tion with chemical reaction mechanism reported by
previous authors[6] .
Acknowledgements
The authors would like to express their appreciation to
Ms. A.Ruhani Mashhadi for AAS tests, Mr. P.Abdollahi
for technical assistance and Mr. S.M.M.Sadrnezhad for
his help in mathematical calculations.
Nomenclatures
b: stoichiometric coefficient (dimensionless)
cA : concentration of H+ ion in the bulk solution (mol/L)
De : effective diffusion coefficient of ions in porous medium
(cm2 /s)
ρa : molar density of the alloy
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R0 : initial radius of particles (microns)
t: time (s)
τ : time for complete conversion (s)
T : temperature (K)
x: fraction extracted