Hydrornetallurgy, 13 (1985) 327--343 327

Elsevier Science Publishers B.V., Amsterdam -- Printed in The Netherlands

GANGUE MINERAL DISSOLUTION AND JAROSITE FORMATION IN

COPPER SOLUTION MINING

J.H. C ANT ER F OR D , P.T. DAVEY and G. TSAMBOURAKIS

CSIRO Division of Mineral Chemistry, P.O. Box 124, Port Melbourne, Victoria 3207
(Australia)
(Received May 4, 1984; accepted in revised form October 15, 1984)

ABSTRACT

Canterford, J.H., Davey, P.T. and Tsambourakis, G., 1985. Gangue mineral dissolution
and jarosite formation in copper solution mining. Hydrometallurgy, 13: 327--343.

The formation of solid reaction products has been recognized as a potential problem
in solution mining operations, but little evidence has been reported on the extent of
precipitation or on gangue mineral degradation. The present study is particularly con-
cerned with the reactions of gangue minerals during the acid dissolution of non-sulphide
copper minerals. Jarosite and gypsum are the major precipitates that form and evidence
is presented that potassium- and calcium-bearing minerals provide the cations for pre-
cipitate formation. Reaction is most pronounced with weathered and/or hydrothermally
altered rock types and can lead to extensive physical degradation of the rock. In a con-
fined environment these reactions could have a deleterious effect on permeability, and
thus on process liquor flowrate and contact with ore minerals. The loss of permeability
could be such that the production rate becomes uneconomical.

INTRODUCTION

Major factors that control the efficiency of solution mining operations

are the relatively unrestricted flow of the leachant/leachate through the
o r e b o d y and adequate contact between the ore minerals and the leachant
[1--3]. Both of these factors are, to a large extent, determined by the
permeability of the orebody. At the c o m m e n c e m e n t of solution mining,
the necessary permeability may be a natural property of the orebody, for
example, gold in a gravel wash, or it may be created by blasting. As solution
mining proceeds, the permeability may increase because of dissolution
of the ore minerals, but also may decrease because of decrepitation effects
or the precipitation of a wide range of reaction products. The loss of perme-
ability may be sufficient to make the rate of production uneconomic,
although before this stage is reached, re-creation of permeability, particular-
ly by pattern blasting, would normally be attempted. Very recently, Prosser
and Roach [4] have developed a mathematical model to account for the
effects of reduced permeability on the rate of a surface chemical reaction.

0304-386X/85/$03.30 © 1985 Elsevier Science Publishers B.V.

328

On the other hand, Letowski [5, 6] has developed a model to account for
the effects of increased permeability as a result of significant dissolution
of non-ore minerals.
Other mineralogical factors that can affect the productivity of a solution
mining operation are the adsorption of dissolved metal cations by existing
sheet silicate minerals, and the formation of secondary minerals [7, 8].
An example of the latter is the formation of secondary malachite by the
reaction of dissolved copper with calcite.
Precipitation of ferric iron has long been recognized [9] as a major
cause of the loss of permeability in m a n y copper sulphide dump anal heap
leaching operations. Although a wide range of ferric precipitates has been
identified, potassium jarosite appears to be the most common. There have
been numerous studies on jarosite precipitation in dump and heap leaching
operations, the most detailed and recent being the theoretical studies of
Liddell and Bautista [10, 11]. The general conclusion is that it is impos-
sible to prevent jarosite precipitation. This is not surprising since jarosite
is often found as a product of the natural weathering (oxidation) of sul-
phide deposits [12, 13]. Jarosite is also known [14] to be a product of the
interaction of sulphuric acid with iron-bearing silicate minerals and may
even form as a primary mineral [15]. The problem of jarosite precipitation
tends to be c o m p o u n d e d by the fact that cementation on scrap iron is the
c o m m o n m e t h o d of copper recovery. That is, the copper recovery m e t h o d
provides a continuous source of ferric iron.
Gypsum and gel-like silica products are among other precipitates that
can form in solution mining operations. Since non-transition metal cations
are normally required for precipitate formation, it is clear that gangue
mineral dissolution must be a major source of these cations. Despite the
fact that gangue mineral dissolution has been recognized [7, 8, 16] as a
major potential problem in solution mining, leading to both loss in perme-
ability and excessive reagent consumption, very few studies have been
directed at quantifying the problem. Probably the most significant study
is that of Riese and Popp [17] who have shown theoretically and experi-
mentally that the degree of interaction between process solutions and
barren country rock is a function of modal composition. Moreover, they
have concluded that excessive reagent consumption, as well as precipita-
tion and permeability losses can be reduced if the leach solution is in equi-
librium with the host-rock minerals but in disequilibrium with the ore-
forming minerals.
In association with a small-scale experimental copper solution mining
operation in South Australia [18, 19], a series of laboratory-scale tests
is being carried out to assist with the determination of the leaching
chemistry and to account for a number of field observations. Some of
these observations can be summarized as follows:
(a) Leaching was occurring to a very large extent in the oxidized ore zone
(copper principally present as cuprite, chrysocolla and malachite). The
 329

rate of leaching appeared to be affected both by the high salinity of

the mine water (chloride = 12--20 g/L, sulphate = 8--20 g/L) and by
the ferric ion present as a result of oxidation of the recycled cementa-
tion circuit outflow.
(b) For every tonne of copper recovered in the cementation circuit, mass
balance calculations indicated that about 0.75 t iron and 3 t sulphate
had precipitated in the underground workings.
(c) There was considerable evidence from chemical analysis of process
streams that there was substantial degradation of rock-forming minerals.
The implications of these and other observations in relation to the long-
term productivity of the operation have y e t to be determined, but from
experience elsewhere it is not unreasonable to suggest that they will proba-
bly be significant.
Four types of solids are being studied in the laboratory-scale leaching
tests:
(i) The major country rock types (amphibolite, gneiss, biotite schist,
pegmatite) recovered either from a diamond-drill core drilled to inter-
sect the primary sulphide zone beneath the underground workings or
from dumps of waste rock.
(ii) Percussion cuttings of sulphide ore from the supergene zone.
(iii) Lumps of low-grade oxide ore recovered from surface stockpiles.
(iv) Crushed samples of high-grade oxide ore and of tailings.
This paper is concerned with some of the reactions of type (i) samples.
An important point to note with the samples used in the present study is
that they are free of sulphide minerals. Details of the dissolution of the
copper from each of the sample types will be presented at a later date.

EXPERIMENTAL

Materials

The mineralogical descriptions of the 4 samples discussed in this paper

are as follows:
Sample A: Biotite amphibolite. A medium- to fine-grained rock with
biotite defining the schistosity. Actinolite--tremolite and biotite are the
major phases, with minor amounts of chlorite, quartz and oligoclase. The
sample was in the form of split diamond-drill core. For some of the leach
tests, crushed core (90% --150 pm) was used.
Sample B: Weathered biotite--chlorite schist. Well developed schistosity,
the major phases being oligoclase, biotite, chlorite and quartz. Several
small malachite veins, up to 2 mm thick and a few centimetres long, were
visible to the naked eye. The lump sample was cut in half and the flat sur-
faces so obtained were polished on a diamond lap.
Sample C: Altered schist. A fine-grained, soft rock, with well developed
schistosity and no visible copper mineralization. The altered nature of the
330

sample was reflected by its high kaolinite content. Pyrite in the original
schist was totally converted to hematite/goethite. This sample was prepared
as in the previous case.
Sample D: Pegmatite. A coarse-grained rock with dominant feldspar
(orthoclase and plagioclase) and quartz, and smaller amounts of muscovite
and biotite. The lump sample was prepared for leaching using the technique
outlined for Sample B.

Leach liquor

Each sample was leached in two different liquors. The first (liquor I)
was discharge (spent) liquor from the cementation circuit [18, 19] and
contained (g/L): Cu 0.003, Fe 0.240, Ni 0.002, Co 0.012, Na 8.59, K
0.055, Mg 2.00, Ca 0.738, A1 0.001, Si 0.011, C1 14.8, and SO4 8.50. The
pH of the spent liquor was 2.83; this was adjusted to 2.00 by addition of
0.5 M sulphuric acid at the c o m m e n c e m e n t of the leaching test. The second
leachant (liquor II) was spent liquor to which solid ferric sulphate was added
to give iron and sulphate contents of 3.91 and 17.9 g/L, respectively. As
with the other liquor, the pH was adjusted to 2.00 at the c o m m e n c e m e n t
of leaching.

Leaching technique

With the exception of the flat, polished face, each solid sample was
painted with an acid-resistant coating (Epicraft polyurethane lacquer) so
that leaching occurred only on a face of known surface area. Each sample
was suspended on terylene cord in a sealed plastic jar containing 1.25 litre
of leach liquor and a magnetic stirrer bar, in such a way that the exposed
face was vertical. The liquor was gently agitated and was sampled at regular
intervals by withdrawal of 2 mL of liquor. The frequency of sampling varied
from sample to sample according to the observed rate of reaction. The pH
of the reaction liquor was maintained at 2.00 by the addition of 0.5 M
sulphuric acid. At the completion of the leach period (14--300 days), the
samples were removed from the vessels, washed with distilled water and
dried in air at ambient temperature prior to mineralogical examination.
The unreacted face of the split sample was used for comparison purposes.
Fresh faces were prepared for treatment in liquor II.
Several leach tests were carried out using crushed Samples A and D.
Twenty-gram grab samples were slurried with 500 mL of leach liquor (ad-
justed to pH 2.00) and agitated with a glass turbine impeller at a rate that
kept all solids in suspension. The reaction vessel was closed to prevent
evaporation losses. The pH of the slurries was continuously monitored and
adjusted as necessary with 0.5 M sulphuric acid. At the end of the leach
period (18 days), the residues were removed, washed with distilled water,
dried in air at room temperature, and mineralogically characterized.
 331

All leach tests were carried out at ambient temperature (15--22°C). Acid
consumption and copper dissolution data were corrected for the volume
changes made throughout each leach period.

Mineralogical analysis

All samples and reaction products were characterized by a combination

of X-ray diffraction, optical microscopy and electron microscopy (JEOL
JSM-25S III and Cambridge Stereoscan scanning electron microscopes and
JEOL JXA-50A electron microprobe).

RESULTS AND DISCUSSION

Sample A

After immersion in liquor I for 27 days, the solid core sample (exposed
surface area = 27.7 cm 2) showed no apparent mineralogical changes and
there was only a nominal amount of acid consumed over this period. Within
3 days of immersion in liquor II, reaction on the exposed surface was ap-
parent. A globular yellow precipitate was seen to be growing o u t from the
surface, while substantial pits developed parallel to the schistosity. At the
same time, the leachate became quite cloudy and a small amount of yellow

i |
| i

Fig. I. Reaction pits and products on exposed surface of Sample A after 14 days immer-
sion in liquor II (ferric-containing spent liquor).
332

Fig. 2. Exposed biotite flakes in pits on exposed surface of Sample A after 14 days
immersion in liquor II (ferric-containing spent liquor).

solid was found in the b o t t o m of the container. Figure 1 shows the core
after 14 days of reaction.
Under the optical microscope it could be seen that the reaction pits were
formed by dissolution of biotite; the b o t t o m s and walls of the pits con-
sisted of flakes of biotite (Fig. 2), many of which expanded and split along
the cleavage planes as a result of the chemical attack. The yellow precipitate
formed mainly on the original sample surface b u t it was also observed in
some pits.
X-ray diffraction and electron microscopy, combined with Energy Disper-
sive X-ray Analysis (EDS), showed that the yellow surface and dislodged
product was jarosite. Figure 3 is a backscattered-electron (BSE) image of
the microcrystalline jarosite on the sample surface. Semi-quantitative
analysis gave the following composition (%): K 7.50, Fe 32.3, S 11.8. These
compare with the theoretical contents (%) for KFe3(SO4)2(OH)6: K 7.81,
Fe 33.45, S 12.80. At this time it is not possible to conclude whether the
low measured data are a result of the semi-quantitative technique used or
a reflection of the known [20] deficiency of K and Fe in many jarosites.
No sodium was detected in the jarosite, indicating a sodium c o n t e n t less
than the detection limit (0.8%) of the SEM used.
As would be expected, the crushed samples were more reactive than the
massive sample. After 18 days in liquor I, the total acid consumption
 333

Fig. 3. BSE image of jarosite formed on surface of Sample A after immersion in liquor
II (ferric-containing spent liquor). White bar = 10 urn.

a m o u n t e d to 12 g H2SO4/kg sample. However, there were virtually no

changes in the mineralogical composition of the sample, as deduced by
XRD analysis. In the ferric solution (liquor II), no acid was consumed;
in fact, the pH d r o p p e d slightly, probably a result of the acid f o r m e d by
j arosite precipitation [ 11 ].

K ÷ + 3 Fe 3÷ + 2 HSO~ + 6 H20 -* KFe3(SO4)2(OH)6 + 8 H ÷

X-ray diffraction analysis of the leach residue indicated the presence of

jarosite, as well as significant reductions in the intensities of the biotite
reflections relative to those of quartz when c o m p a r e d with the original
sample. There were less marked decreases in the intensities of the oligoclase
reflections. These effects indicate that the biotite cont ent , and to a lesser
e x t e n t the oligoclase c o n t e n t , of the residue is lower than t hat of the original
sample, and would suggest that partial dissolution of these c o m p o n e n t s
has occurred.
334

Fig. 4. Elongated crystals of gypsum growing out of the surface of Sample B after 292
days immersion in liquor I (spent liquor). In the upper photograph the large elongated
grain is Ca-rich plagioclase.
 335

Sample B

In liquor I, rapid reaction was observed to take place. The small malachite
veins were seen to be dissolving, while there was significant outgrowth of
elongated crystals of gypsum from the reacting surface (Fig. 4). This growth
was most pronounced around the perimeters of the large Ca-rich plagioclase
crystals and several cracks. A slice of sample, 8 mm thick and parallel to
the leached face, was removed and split in half at right angles to the leached
face. Under the optical microscope it was quite clear that the leach liquor
had penetrated to a depth of about 7 mm, dissolving out the malachite.
The zone closest to the leached face was covered by gypsum crystals. To-
wards the limit of leachant penetration, there was significant "iron-staining".
This was shown to consist of well formed jarosite and gypsum crystals
(Fig. 5) with some apparently amorphous iron-rich solids (Fig. 6).

Fig. 5. BSE image of jarosite and large tabular gypsum crystals f o r m e d at limit of leachant
p e n e t r a t i o n on Sample B after 292 days immersion in liquor I (spent liquor). White bar =
100 ~m.
336

Fig. 6. BSE image of iron-rich crust and biotite flakes f r o m limit of leachant penetration
on Sample B after 292 days immersion in liquor I (spent liquor). White bar = 100 u m

Over the 292-day leaching period, a total of 64 mL of 0.5 M sulphuric

acid was added to maintain the pH at 2.00. The amount of copper leached,
the rate of which was approximately linear, was 55 mg/cm 2. Analysis of the
final liquor, after removal of the small amounts of solid crystalline jarosite
and gypsum, gave the following composition (g/L): Cu 0.579, Fe 0.282,
Ni 0.013, Co 0.045, Na 8.29, K 0.142, Mg 2.00, Ca 0.735, A1 0.091, Si
0.064, C1 15.0, SO4 11.0. Comparison with the composition of the starting
liquor clearly indicates that dissolution of Cu--Co--Ni-bearing minerals and
silicate minerals has occurred. For example, the cobalt, aluminium, potas-
sium and silicon contents have increased by factors of ~4, ~90, ~2.6 and
6, respectively.
Reaction with liquor II (ferric-containing spent liquor) was rapid and
pronounced. The surface became coated with a yellow precipitate (shown
to be jarosite) and fine elongated gypsum crystals, while there was signifi-
cant swelling and cracking (Fig. 7). No acid addition was required to main-
 337

Fig. 7. Jarosite precipitation and swelling and cracking of leached surface of Sample B
after 90 days i m m e r s i o n in liquor II (ferric-containing spent liquor).

tain the pH at 2.00. For the first 60 days the rate of copper minerM dis-
solution was approximately the same as the in iron-free liquor I, although
the actual amount of copper leached was about 20% higher.* Over the
next 30 days, the copper dissolution rate increased rapidly; after 90 days,
the amounts of copper dissolved were 35 mg/cm 2 and 21 mg/cm 2 for liquors
II and I, respectively. This increase probably resulted from the exposure
of extra copper mineralization by the pronounced swelling and cracking.
Examination of a cross-section of the sample supported this conclusion.
A considerable amount of jarosite and gypsum was dislodged from the
surface of the sample during leaching, and this was removed from the leach-
ing vessel before analysis of the final liquor. After 90 days reaction, this
had the following composition (g/L): Cu 0.420, Fe 3.27, Na 8.78, K 0.003,
Mg 2.12, Ca 0.748, A1 0.058, Si 0.032, C1 15.1, SO4 17.1. There was a
substantial reduction in the potassium concentration, a less marked reduc-
tion in the sulphate concentration, while there were increases in the alumini-
um and silicon concentrations. The reduction in the potassium concentra-

*Accurate correlation of the two leaching rates is not possible because of differences
in the a m o u n t of copper mineralization exposed on the leached surface.
338

tion from 0.055 to 0.003 g/L could not account for the amount of jarosite
precipitated. The bulk of the potassium required for jarosite precipitation
must, therefore, have come from the acid degradation of some of the potas-
sium-containing minerals in the sample. Dissolution of calcium-containing
minerals would provide the calcium ions required for the observed gypsum
precipitation.

Sample C

After 104 days immersion in liquor I (spent liquor), the most noticeable
changes to this sample were cracking and the formation of small, white,
tabular crystals, particularly around the edges. X-ray diffraction analysis
showed these crystals to be gypsum. Gypsum crystals were also observed
in many of the cracks. The surface had also become roughened. At the
end of the leach period, the liquor had the following composition (g/L):
Cu 0.475, Fe 0.275, Ni 0.003, Co 0.033, Na 9.82, K 0.102, Mg 2.36, Ca
0.731, A1 0.064, Si 0.064, C1 17.2, SO4 11.9. Although, as noted previous-
ly, there was no apparent visible copper mineralization, the amount of
copper dissolved after 104 days was equivalent to 56.6 mg/cm 2. A total of
15 ml of 0.5 M sulphuric acid was required to maintain the pH at 2.00.
In liquor II (ferric-containing spent liquor) reaction of Sample C was
quite spectacular. After 10 days, significant cracking developed and exfolia-

Fig. 8. Sample C after 20 days immersion in liquor II (ferric-containing spent liquor).

 339

Fig. 9. Sample C after 90 days immersion in liquor II (ferric-containing spent liquor).

tion commenced; Figures 8 and 9 show the exposed surface after 20 and 90
days, respectively. The cavity formed was approximately 15 mm deep. A
considerable volume of the original material that broke away from the
sample underwent reaction; the solids in the b o t t o m of the reaction vessel
also contained jarosite. Over the 90-day reaction period the pH of the
liquor fell to 1.49. The concentration (g/L) of the final liquor was as fol-
lows: Cu 0.258, Fe 2.57, Na 10.4, K 0.0003, Mg 2.40, Ca 0.804, A1 0.060,
Si 0.051, C1 17.2, SO4 17.3. As with Sample B, these analytical data are
indicative of substantial degradation of the minerals making up Sample C.
Despite the swelling, cracking and exfoliation, the a m o u n t of copper dis-
solution in the iron~ontaining liquor II was less than that observed in the
iron-free liquor (I) -- 26.5 mg/cm 2 compared with 51.1 mg/cm 2. It is not
known if this reduction is due to a reduction of the area of exposed copper
mineralization by the jarosite precipitated, or was due to a reduction in
the actual a m o u n t of copper mineralization within the body of the sample.

Sample D

Of the four samples presently under discussion, this was the least reac-
tive. Immersion of the exposed face of the solid core in spent process liquor
at pH 2.00 in the absence (liquor I) and the presence (liquor II) of ferric
iron did n o t result in any significant changes to the exposed mineral con-
340

stituents. For the crushed core sample, acid consumption in liquor I was
equivalent to 17 g H : S O J k g sample after 18 days. In liquor II (ferric-
containing spent liquor), X-ray diffraction analysis showed the presence
of traces of jarosite. Under the optical microscope, a number of the feld-
spar grains appeared to have undergone surface reaction; the grain surfaces
showed noticeable "roughening".

GENERAL COMMENTS

The results of the present study clearly indicate that acid degradation of
rock-forming minerals can be substantial, particularly in the presence of
ferric iron. The reactions occur quite rapidly over a time scale that is relevant
to solution mining. The most reactive rock types are those that are highly
weathered or hydrothermally altered. In the present case, the two pre-
dominant precipitates formed are gypsum and jarosite. In addition, the
concentrations of, for example, aluminium and silicon, in the process liquor
are significantly increased. Although the process liquor used in the present
study has a high sodium content (8.59 g/L) and a low potassium content
{0.055 g/L), the jarosite formed is apparently sodium-free. This is con-
sistent with the known [21] greater stability of jarosite compared with
natrojarosite. Thus the following ambient temperature data have been
reported:

KFe3(SO4)2(OH)6 + Na ÷ -~ NaFe3(SO4)2(OH)6 + K ÷

log a K . /aNa÷ = --3.92

In view of the low potassium content of the process liquor, the source of
the potassium required for jarosite precipitation can only have come from
potassium-containing minerals in the samples. Ivarson, Ross and Miles
[22--24] have shown that feldspars, micas and other silicate minerals play
an important role in the microbiological formation of jarosite-type minerals
in soil environments.
According to Loughnan [ 2 5 ] , chemical weathering studies of a range
of rock types can be interpreted in terms of the following simplified increas-
ing mineral stability series:

Olivine, Ca-plagioclase
Augite
Hornblende Increasing
Biotite, Na-plagioclase stability
K-feldspar
Muscovite
Quartz

As stated previously, evidence was obtained of extensive biotite dissolution.

 341

Degradation of K-feldspar and Ca, K-feldspar would provide additional

potassium ions. Much of the calcium required for gypsum precipitation
has probably been derived from the Na, Ca-feldspar.
The actual mechanisms of degradation are exceedingly complex, depend-
ing upon numerous factors, particularly pH and redox potential. Thus one
mineral may break down via more than one route. For orthoclase, the fol-
lowing reactions are known [26] to occur:
2 KAISi3Os + 2 H÷ + 9 H20 -+ H4AI2Si209 + 4 H4SiO4 + 2 K+

orthoclase kaolinite

3 KAISi308 + 2 H+ + 12 H20 -+ KAI3Si30,0(OH)2 + 6 H4SiO4 + 2 K+

orthoclase illite

Numerous structural changes occur, and some of these involve a volume

expansion [26].
From a solution mining point of view, the ready dissolution of calcium
and potassium from rock-forming minerals is undesirable because it provides
the cations necessary for the precipitation of gypsum and jarosite. Under
the initially acidic conditions, aluminium and silicon dissolution are likely
to be substantial and there is the possibility that these can reprecipitate
in bulky hydrated forms such as new clay minerals [26]. Moreover, the
possibility of incorporation of, in the present case, copper ions into the
precipitate cannot be ignored.
The present study does not provide any information as to the loss, if
any, of the permeability in a "real" environment and what effect this would
have on mineral--leachant contact and leachant flowrate. Column leaches
are now being carried out to ascertain this information. Additional tests
are being carried out with mono-mineralic samples to establish an order
of rock-forming mineral reactivity under conditions appropriate to solu-
tion mining. Another factor being examined is the effect of the salinity of
the leachant on the relative reactivities. What can be said unequivocally at
this stage, however, is that jarosite formation in solution mining opera-
tions can occur to an appreciable extent in the absence of sulphide minerali-
zation, an observation that does not appear to have been previously com-
mented upon despite the fact that hypogene jarosites are known [15].
Obviously there needs to be a source of ferric iron; in virtually all copper
solution mining operations the copper is recovered by cementation with
scrap iron. It is the aqueous iron so formed that acts as a source of iron
for jarosite formation even if there is no soluble iron present as a result
of pyrite oxidation [ 1].
342

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