Minerals Engineering, Vol. 12, No. !, pp.

93-106, 1999
© 1998 Elsevier Science Ltd
Pergamon All rights reserved
0892--6875(98)00122-8 0892-6875/99/$ - - see front matter

BIOLEACHING OF A SPANISH COMPLEX SULPHIDE ORE

BULK CONCENTRATE

C. GOMEZ, M.L. BL.~,ZQUEZ and A. BALLESTER

Dpto. de Ciencia de Materiales e Ingenierfa Metaldrgica, Facultad de Ciencias Qufmicas,

Universidad Complutense, 28040 Madrid, Spain. E-mail: cgcastro@eucmos.sim.ucm.es
(Received 28 November 1997; accepted 10 August 1998)

ABSTRACT

In the present work the applicability of bioleaching using a mixed culture of mesophilic
microorganisms (Thiobacillus ferrooxidans, Thiobacillus thiooxidans and Leptospirilum
ferrooxidans) on a bulk concentrate of a Spanish complex sulphide ore was studied. The
bulk concentrate mainly consisted of by chalcopyrite, sphalerite and pyrite. Effects of
nutrient medium, stirring, pulp density, temperature and the addition of CO2 (1% v/v) to
the airflow were also studied. The highest leaching rates and recoveries were obtained
with mechanically stirred reactors at 5% pulp density and 9K medium. However, by using
9K medium higher jarosite precipitation was observed. Results showed that the optimum
temperature for copper bioleaching was 30°C, whereas zinc dissolution increased with
a rise in the temperature. © 1998 Elsevier Science Ltd. All rights reserved

Keywords
Sulphide ores; bioleaching; extracive metallurgy

INTRODUCTION

A complex sulphide is an association of chalcopyrite, sphalerite and galena disseminated in a pyritic matrix.
As well as copper, zinc and lead as valuable metals, such deposits may contain significant quantities of
silver, gold, arsenic, antimony, bismuth and mercury. Numerous deposits of these ores exist in the world
(Australia, Canada, Portugal, Spain, etc). It is estimated that Spanish complex sulphides contain 70 % of
the reserves of these valuable metals belonging to the European Union Countries; the Spanish reserves are
approximately 250 million tons, which gives an idea of their economical importance [1].

Complex ores are often characterised by particularly fine intergrowth of the mineral values. For instance,
chalcopyrite and sphalerite are frequently intergrown, micro-size grains of 10-20 lma being dispersed within
the pyrite. Due to these specific mineralogical characteristics, it is necessary to finely grind and concentrate
the ore prior to the solubilisation of the valuable metals [2]. To obtain separate concentrates (of Cu, Zn and
Pb) by selective flotation involves high unit-cost, poor quality of the concentrates and relatively low overall
recoveries. To obtain bulk concentrates by bulk flotation in which the non-ferrous sulphides float together
and are separated from the pyrite, it is more economic if a hydrometallurgical process is applied [3].

One alternative for the treatment of bulk flotation concentrates is bacterial leaching [4]. Microbiological
processes use the ability of chemolithotrophic autotrophic bacteria, such as those belonging to the genus

93
94 C. G6mez et al.

Thiobacillus, to oxidise metallic sulphides and elemental sulphur into water-soluble sulphates. Especially
remarkable are the species Thiobacillus thiooxidans and Thiobacillusferrooxidans which oxidise inorganic
sulphide and other reduced valency sulphur compounds to sulphate and sulphuric acid. Accordingly it can
be written:

T.ferrooxidans, T.thiooxidans
S° + H20 + 3•202 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . > H2SO 4 (1)

However, the more important role in the bacterial leaching processes is played by Thiobacillusferrooxidans.
These bacteria, apart from the above mentioned oxidation reaction (1), are able to oxidise Fe 2* to Fe 3+. The
ferric ion is known to be an effective oxidising agent and it further contributes to the dissolution of
sulphides.

In the past, bioleaching on a number of sulphide minerals, such as sphalerite, chalcopyrite, pyrite,
molybdenite, etc. have been extensively studied [5,6]. However, little work on bioleaching of complex
sulphides has been done [7,8]. Thus, the aim of this paper is to study the applicability of a bioleaching
technique to a bulk concentrate of a Spanish complex sulphide, obtaining the optimal conditions for the
dissolution of the metal values.

EXPERIMENTAL

Mineral

The bioleaching experiments were carried out with a bulk concentrate of a Spanish complex sulphide ore
obtained by continuous flotation in a pilot plant. It was provided by Rio Tinto Minera, S.A. (Huelva, Spain).
Its chemical and mineralogical compositions are given in Table 1. Chemical analysis was carried out by
Atomic Absorption Spectrometry (AAS), except for arsenic which was determined by a colorimetric method.
X-ray diffraction showed sphalerite (ZnS), chalcopyrite (CuFeS2) and pyrite (FeS2) to be the major phases
in the bulk concentrate. To determine the mineralogical composition it has been assumed that iron is
stochiometrically present in chalcopyrite and pyrite, and in substitutional positions in 5% of the zinc sites
of the sphalerite lattice. The granulometric analyses were carded out in a cyclosizer and indicated that the
particle size of the complex sulphide concentrate was 80% below 30 pm.

TABLE 1 Chemical and mineralogical composition of the bulk concentrate

Zn Pb Cu Fe As

Chemical composition (%) 17.1 1.7 14.0 25.0 0.12

Sphalerite Galena Chalcopyrite Pyrite

Mineral phases (%) 27.7 2.0 40.4 24.3

Bacteria

A mixed culture of iron- and sulphur-oxidising microorganisms, whose origin was a Rio Tinto mine water,
was used. Characterization of this culture showed that the main bacteria strains were Thiobacillus
ferrooxidans, Thiobacillus thiooxidans and Leptospirillum ferrooxidans. The culture was originally enriched
in shake flasks using a chalcopyrite concentrate (5% wt/vol.) as substrate. The conditions for bacterial
growth in a 9K medium modified without iron [9] were as follows: 35°C, 160 rpm and pH 1.8. The
 Bioleaching of a Spanish complexsulphide ore 95

bacterial culture were tested by assessing their acid production and microscopic cell counting in a Thoma's
chamber. When the culture was in the exponential growth phase (around l0 s bacteria/ml) a sample was
taken to inoculate a bioleaching experiment.

Bioleaehing experiments

In order to optimize the bioleaching process, nutrient medium, stirring, pulp density, temperature and CO 2
addition (1% v./v.) to the air flow were studied. When the influence of one of them was studied the rest
were fixed at the conditions shown in Table 2.

T A B L E 2 Composition of the used nutrient media

Variable Tested conditions Fixed conditions

Nutrient medium Tap water, D1, D2 and 9K 160 rpm, 35 *C, 5% pulp

medium density, CO2 addition (1%

v./v.) to the air flow.

Type of stirring I reactor Mechanically stirred 160 rpm, 35 *C, D1

reactors and orbital shake. medium, 5% pulp density.

Pulp density 5, 10, 15 and 20% pulp 160 rpm, 35"C, D1

density (w/v solid/liquid). medium, CO2 addition (1%

voL/vol.) to the air flow.

C02 addition With and without CO 2 160 rpm, 35 *C, D1

addition to the air flow. medium, 5% pulp density.

Temperature 20, 30, 35 and 40 *C 160 rpm, 35 *C, D1

medium, 5% pulp density,

COz addition (1% v./v.) to

the air flow.

All experiments were carried out in mechanically stirred reactors with 500 ml hemispherical flasks, except
when the influence of the type of reactor was studied. In this case, an orbital shaker with 250 ml shake
flasks was used. Before inoculation, the concentrate was added to the nutrient medium and pH was adjusted
to 1.8 by H2SO 4 addition. The compositions of the nutrient media are given in Table 3. After a leaching
period of 2 hours, 5 ml of bacterial culture per 100 ml of solution were added to the reactor. Additionally,
in order to compare the effect of the nutrient medium on metal solubilisations, a control test (sterile) was
performed. In this case a solution of thymol (2 % wt) was added in order to kill the microorganisms.

Periodically, when the pH was higher than 1.8, it was adjusted to this value by acid addition. However, if
the pH was lower than 1.8, a free evolution of this variable was allowed. Water losses by evaporation were
compensated by the addition of distilled water. Each experiment was monitored, following the copper, zinc
and total iron concentrations by AAS. Upon termination of the experiments, the leached residues were
96 C. G6mezet al.

washed with sulphuric acid in water at pH 1.8, and analysed by X- ray diffraction in order to identify the
products resulting during bioleaching.

TABLE 3 Tested variables for the bioleaching optimisation

Nutrient salt 9k medium Norris' medium D1 D2

(g/L) (g/L)[10] (g/L) (g/L)

(NH4)2S04 3.0 0.2 0.06 0.01

MgSO4"7H20 0.5 0.2 0.06 0.01

K2HP04 0.5 0.2 0.02 0.01

KCI 0.1 0.02 0.01

Ca(NO3)2-H20 0.01

RESULTS AND DISCUSSION

Influence of nutrient medium

In Figure 1 the influence of nutrient medium on the leaching of copper (Figure la), zinc (Figure lb) and
iron (Figure lc) is shown. Five different media, 9K, Norris, D1, D2 and tap water were tested (Table 3).
None of these media contained Fe 2+, thus preventing the precipitation of j arosites [ 10-12] and ensuring that
the microorganisms obtained their energy from the sulphide minerals. As can be observed, the nutrient
medium strongly influenced both the leaching rate and the copper, zinc and iron extractions. The following
order can be established for the leaching rate (V) : V9K > Vnorris > VDI > V D 2 > V tap water" For "sterile"
tests the metal recoveries remained practically zero at all times. These data have been omitted in the Figures
for the sake of clarity.

It is noteworthy that our results are in agreement with the currently accepted electrochemical mechanism
of explaining the bioleaching of metal sulphides. According to this, the following order of dissolution from
the concentrate could be expected [13]: sphalerite>chalcopyrite>pyrite. Sphalerite is the most
electrochemically active, while the chalcopyrite will behave anodically with respect to sphalerite and
cathodicaily with respect to sphalerite. In all tested media (Figure 1), the above mentioned sequence is
observed; i.e., after the 10th day, in the 9K medium, about 80 % Zn, 30 % Cu and 20 % Fe are dissolved.
 Bioleachingof a Spanish complexsulphideore 97

40 -]
oo O_-O O_o. '"1
--O--gKmedium _ ,., 1~,1

... 20 J -a--v2 m.ium / t X l X ~ ~ I

l-°-="r //x I
10" ~ ~J I Q ~ l

80 | I

0
50
40
~ 30
~ 2o

(d)

2.o
1.5

0 2 4 6 8 10 12 14 16 18 20 22
Time (days)

Fig. 1 Influence of nutrient medium in the leaching of copper (a), zinc (b) and iron (c) and evolution of
pH (d).

The decrease in the leaching rate in the more diluted media (D 2 and tap water) is a consequence of a lower
bacterial activity, as can be followed from the iron evolution (Figure lc). As is well known, a minimum
concentration of basal salts is necessary to obtain a good bacterial activity and metals solubilization. As can
be seen in Figure 1, the optimum medium of those investigated for the growth of microorganisms is the 9K
medium. However, its main drawback is the high concentration of sulphate, ammonium and potasium ions,
which produce the precipitation ofjarosites [12], which have been detected by X-ray analysis of the residues
in the 9K medium in this work. No traces of jarosite were observed in other media.

A better bacterial activity in the 9K medium, compared with the other media, can be seen in Figure ld,
which is seen in the pH evolution. In all cases, an initial increase in pH, attibuted to the chemical
dissolution of the concentrate, was observed between 0 and 3 days. However, after the eighth day in the
9K medium, a strong decrease in the pH of the solution was observed. This decrease in pH is not produced
in the other media, in which the pH remained almost constant between 2.0 and 2.3. Two reasons can
98 C. G6mez et al.

account for this decrease in pH, a great bacterial growth (Eq. 1), detected by microscopic observations, and
a precipitation of jarosites according to:

3Fe 3+ + X + + 2HSO4- + 6H20 ~ XFe3(SO4)2(OH) 6 + 8H ÷ (2)

where X= K +, Na ÷, NH4 ÷ and H3 O÷.

Influence of the type of reactor/stirring

To study the effect of stirring two types of reactors were used: mechanically stirred reactors and shake
flasks. In Figure 2, copper (Figure 2a), zinc (Figure 2b) and iron (Figure 2c) dissolution for both reactors
can be observed. The highest rates and yields were obtained with mechanically stirred reactors.

40
--A-- Mechanical stirring ~ A . . . . . . A _ . . . _ A ~ A (a)
30 --D-- Shake flasksA..~..A

20 d .-----El
0
10

0 ~ ~ , I , t , I , t . I . I . I . I ,
80 A---'---A"~''A A (b)
60

40
o/
2O - ~~._~_~/o ~°
0
50
4O
~ 30
,? 20
10

0 J=.._,_~~,.,---:. ~ , . , . , . , . , . , . ,
0 2 4 6 8 10 12 14 16 18 20 22
Time (days)

Fig.2 Influence of type of reactor/stirring on the leaching of copper Cu (a), zinc (b) and iron (c). Sterile
recoveries were always lower than 1% for all metals.

A kinetic study was carried out in order to determine the rate-controlling step of the bioleaching reaction.
Thus. the obtained data were fitted according to the shrinking core product layer model for heterogeneous
 Bioleaching of a Spanish complex sulphide ore 99

reactions [14]. As already mentioned, during bioleaching both sulphur (produced in the oxidation reaction
of mineral sulphides) and jarosites (equation 2) were formed as two insoluble products, which form a
product layer over the mineral sulphides. In such conditions, if the leaching rate was controlled by diffusion
through these products, the following equation rate would apply [14]:
2
1 - 2R-(l-R) 3'-- Kpt (3)
3

where R=fraction reacted, t=time (day) and Kp=parabolic rate constant (day-l).

However, if the chemical reaction was the controlling step of the reaction the following rate equation would
apply [15] :
1
1- (1- R) 3 : kt (4)

Figure 3 shows that copper and zinc leaching follow a mathematical law such as (4) for data in the bacterial
exponential growth. That is to say, the chemical reaction is the controlling step of the reaction and not the
diffusion through the layer. The K values for copper and zinc calculated from Figure 3 are shown in Table
4. As can be seen, the rate of zinc dissolution is faster than the rate of copper dissolution and better kinetics
were obtained in mechanically stirred reactors.

0.25
I'~ ~// zx Mechanical stirring
0.20

0.15
1.-

n,"
I
0.10
"7"
0.05

0.00 I = I i I t I i I

0.10

0.08

0.06
fieI
%.,...
"v 0.04

0.02

0.00 /
I = I = I = I I I
100 150 200 250 300
Time (h)
Fig.3 Plots of 1 - ( l - R ) v3 versus bioleaching time for copper (a) and Zn (b) of the bulk concentrate.
100 C. G6mez et al.

TABLE 4 Values of the kinetic constants (h-1) for the copper and zinc bioleaching for shake
flasks and mechanically stirred reactor
Shake flasks Mechanically stirred reactors

Zn 11.7 " 10 "4 26.9- 104

Cu 2.9" 10 "4 4.2 "10 "4

Influence of COz addition

It is well known that autotrophic microorganisms, such as Thiobacillusferrooxidans need a minimum CO 2
concentration [16], since they obtain their cellular carbon from this compound. Figure 4 shows the influence
of the CO 2 addition (1% v/v) on the air flow in the leaching of copper (Figure 4a), zinc (Figure 4b) and
iron (Figure 4c) in mechanically stirred reactors. It can be seen that the leaching rates and extractions of
these metals were similar, irrespective of the CO 2 addition. These results are in agreement with those of
Bruynesteyn who affirmed that the carbon content in the atmosphere can be enough to cover the nutritional
requirements of microorganisms [17].

30. ---O-W~out CO= (a)

--El-- W'dll CO2 _jO~(:~ ^ m
,..., 2 0 ' - - X - - Sterile (with COz) /~...>'~

g 4o
so
0
I
Ill. ~ X ,

j -Y°
, . ~::~--:l<-TN . - - ; ~ r - ~ < 7 - . x , ¥-T--:-.X,
(b)

20

0 .r'~;--T-;--~<:~--~:--:-:~ .--:--r--,x-r-¥ , ¥-r-rX, .

15 ....~Ooj..~O (C)

,-.10 ~ ~ ~i ~ . , .x
6

-r-.X , ,xT--;-,x,
0 2 4 6 8 10 12 14 16 18 20 22
Time (days)

Fig.4 Influence of the C O 2 addition on the copper (a), zinc (b) and iron (c) bioleaching.
 Bioleaching of a Spanish complex sulphide ore 101

Influence o f pulp density

The influence of pulp density, ranging from 5 to 20%, is shown in Figure 5. A significant decrease in both
bioleaching rate and extractions of copper (Figure 5a), zinc (Figure 5b) and iron (Figure 5c) were observed
when the pulp density was increased, being maximum for 5% pulp density. The decrease in the percentage
of metal dissolution when the pulp density is increased would be due to a lower availability of oxygen and
CO2, which are essential nutrients for ThiobaciUus ferrooxidans growth. Our results agree with those
observed by Chaudhury and coworkers on Cu-Pb-Zn complex sulphides [18] and zinc concentrates [19].

3O
•
-o- s~p.d. (a)
25 - -o- 10% p.d. j...C3~E3 []
• --A-- 15% p.d. J 3 " " -
20- --0-- 20% p.d.
15 " - x - Sterile (5% p.d.) . . ~

,-,- /:..7 .,~ °~° (b)

/ u = _O_...91~.___A__A
• / ....O ~ ^.----~"-'=

0- ~ ,s,=~IC--~-T-T-.x-T-xTx~-. >p-:-~.

'°i I
40 ~9.~-~- ~--A
20

0-~ ~ ~

1o. I
5" ~[:f...-O~....-A--A-----A--A I

0 2 4 6 8 10 12 14 16 18 20 22 24
Time (days)

Fig.5 Influence of pulp density on the copper (a), zinc (b) and iron (c) bioleaching.

In order to relate the pulp density to the metal extraction, which directly depends on the bacterial
concentration, a kinetic study has been performed. According to the model proposed by Michaelis-Menten
[20] the dissolution rate is given by the following equation:
102 C. G6mez et al.

V.S
V -- m (6)
(Ks+ S)

where V is the extraction rate of metals, V m is the maximum metal extraction rate, S is the pulp density
and K s is the Michaelis' constant. This constant gives an idea about the affinity of the bacteria to the
mineral substrate. In Figure 6 plots of 1/V versus I/S for copper and zinc dissolutions are shown. From
these representations the kinetic parameters V m and KS for copper and zinc dissolutions can be obtained.
Their values are summarised in Table 5. These results confirmed a better zinc than copper dissolution from
the bulk concentrate, because Vm)zn is four times higher than Vm)cu. The higher value of KS)Cu than Ks)zn
might indicate a preference of the microorganisms for the copper from the concentrate.

400
0 Cu
350

300
=

~-~ 250-

"' 200-

,,¢--
150-

100 -

50-

O- ' ' , I , I , I ,
0.000 0.005 0.010 0.015 0.020 0.025
1/S (g.L) 1
Fig.6 Plot of Michaelis-Menten for the copper and zinc dissolutions.

TABLE 5 Values of maximum rate of dissolution, Vm, and kinetic constant, Ks, for copper and
zinc bioleaching

Vm (mg'L'l"h "1) Ks (g.L "1)

Zn 29.7 36.7

Cu 7.3 86.9
 Bioleaching of a Spanish complexsulphide ore 103

Influence of temperature

Figure 7 shows the influence of temperature on the rate of copper (Figure 7a), zinc (Figure 7b) and iron
(Figure 7c) dissolution. A different behaviour in copper and zinc dissolution can be observed. The rate of
zinc leaching increased with a rise in temperature, whereas the copper leaching rate reached its optimum
at 30°C and strongly decreased at 20°C and 40°C. These results could be justified on the basis of two
different mechanisms for copper and zinc dissolutions. Copper could be mainly dissolved by a microbial
mechanism, whose maximum activity is reached at temperatures around 30°C, as can be observed in Figure
7c. However, the behaviour observed for zinc could be associated to a chemical dissolution mechanism,
obtaining better extractions when the temperature is increased.

30 q /O----O o o (a)
1 ~ o - O " ^___._..~--zx----A I

¢~10q
1 /,//'~.0 ~ 6_o~o_o o ~ O / O
I,
0 o~
80
60
40
20
[] 0--------0
0. -r
] (c)I
15 ] ~o -o'°" . / ~ - ' ~ - I

0 . ~ x - - x - - x ~
"---° I
0 2 4 6 8 10 12 14 .16 18 20 22
Time (days)
Fig.7 Influence of the temperature on the copper(a), zinc (b), iron (c) bioleaching.

The Arrenhius plot is a very useful tool for elucidating the mechanism involved and explicitly expressing
the kinetics of a given process [21]. An attempt has been made to calculate the activation energy for zinc
and copper dissolutions using the Arrhenius equation:

-E (7)
K-- A ' e "RT

where K is the rate constant, A is the frequency factor, T is the absolute temperature, E a is the activation
energy and R is the gas constant.
104 C. G6mez et al.

The rate constant, K, was determined assuming that the kinetics of dissolution were controlled by the
chemical reaction. As can be observed, in the Arrhenius plot (Figure 8), In(K) for the zinc dissolution shows
a linear dependence with l/T, while this dependence is parabolic for the copper dissolution. These results
suggest greater importance of the microbial processes in copper bioleaching. However, in the zinc
dissolution a chemical leaching of ferric ion produced could be presumed. From Figure 8 an activation
energy of 110 KJmol -~ has been obtained for the zinc dissolution.

-6.0
a Cu
-6.5. t, Zn

-7.0.

-7.5

~ -6,0 • J''-'-- "~-

C
.-I

-8.5

-g.0-

-10.0 I I i I ,
3 . 1 5 x 1 0 °3 3 . 2 5 x 1 0 .3 3 . 3 5 x 1 0 .3 3 . 4 5 x 1 0 .3

I/T(K -I)

Fig.8 Arrhnenius plot to measure activation energy for copper and zinc leaching. K is given in h-L

CONCLUSIONS

On the basis of the preceeding results the following conclusions can be made:

1. The best leaching rates and recoveries were obtained with 9K medium. However, its use produced
much jarosite precipitation.

2. Copper and zinc dissolutions conform to a shrinkage core-chemical controlled reaction. Faster
kinetics were obtained in mechanically stirred reactors.

3. Copper and zinc dissolutions fit the kinetic model of Michaelis-Menten in the range pulp density
5 to 20%, the optimum being was 5%.

4. The optimum temperature for copper bioleaching was 30°C, while zinc bioleaching leaching rate
increases with a rise in temperature.

5. Kinetic studies suggest that copper dissolution ocurred by a microbial mechanism. However the
zinc dissolution could be associated to a chemical reaction.
 Bioleachingof a Spanishcomplexsulphideore 105

ACKNOWLEDGEMENTS

The authors wish to express sincere gratitude to the Comision Interministerial de Ciencia y Tecnologfa
(Spain) and to the Commission of the European Communities for funding this research through projects
PBT87-0032-C0201 and MA2M-CT90-0028 (SMA), respectively.

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106 C. G6mez et al.

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