ABSTRACT

An experimental system has been designed to monitor on-line

variations of leaching parameters in a closed circuit of cyanide leach-
ing solutions and gold bearing ores. Experiments performed to deter-
mine variations in some important leaching parameters of the solu-
tion: pH, dissolved oxygen, free cyanide, oxidation/reduction poten-
tial, gold content, temperature, pressure and solution chemistry. By
comparing results obtained when the leaching solution is allowed to
become acid or kept basic, it was possible to infer the chemical reac-
tions that occurred between the solution and the ores.
INTRODUCTION
Heap leaching was introduced by the USBM during the late
1960s as an alternative method for treating low grade ores in
Nevada. Since then, many improvements have been made in terms
of materials handling, understanding the cyanide/gold chemistry and
carbon adsorption process (Marsden et al, 1992; Wadsworth et al,
2000; Kirk et al, 1978). Work has also been done on modeling the
transport phenomena in heap leaching pads (Bouffard et al, 2001;
Bartlett, 1997; Sanchez-Chacon et al, 1997). But little work has been
done however in terms of measuring changes in leaching parameters
at a laboratory scale. Typical tests include ore mineralogy, bottle tests,
column leach tests, and pilot-scale leach tests (Yannopoulos, 1991).
These tests are extremely important when determining the feasibility
of gold leaching of a particular ore, but do not give fast results in
terms of parameter changes that may occur when different types of
ores or leaching solutions are used.
Work has been performed on developing industrial scale sen-
sors for cyanide, pH and oxygen determination in leaching pads
(Vorster, 2001) which makes it an incentive to develop a small labo-
ratory scale for fast ore leach tests that will allow predicting changes
at a large scale.
This work presents the results of monitoring online changes in
the leaching parameters of gold bearing ores. Experiments using
ores (with and without lime addition) and cyanide leaching solutions
were performed to determine variations in the important leaching
parameters: pH, dissolved oxygen (DO), free cyanide concentration
([CN
-
]), oxidation/reduction potential (ORP), gold content ([Au]), tem-
perature (T), pressure (P) and final solution chemistry. By comparing
the results obtained when the leaching solution is allowed to become
acid or kept basic, it was possible to propose chemical reactions that
are occurring between the solution and the ore.
EXPERIMENTAL SYSTEM AND PROCEDURE
A reactor was designed and constructed for continuous monitor-
ing of pH, ORP, [CN
-
], DO, temperature and pressure while passing a
cyanide containing solution through an ore sample. A schematic of
the system is shown in Figure 1, it consists of: a column for placing
the ore; a reservoir for the solution; a series of separate small reser-
voirs for placing the electrodes; a peristaltic pump that circulates the
solution through these reservoirs; a peristaltic pump that feeds the
solution to the top of the column; gas sampling ports at the top of the
column and top of reservoir; pressure transducer and thermistor on
top of reservoir; data acquisition system and meters. The system is
hermetically sealed to avoid gases from leaving or entering the sys-
tem.
For monitoring ORP and [CN
-
], a platinum inlay electrode and a
solid-state half-cell electrode was used. Both electrodes were refer-
enced to a Ag/AgCl double junction electrode. To determine dissolved
oxygen (DO), a galvanic type electrode was which does not require
special heating to measure.
50 and 100 ml gas samples were taken for HCN, NO2, NH3 and
O2 analysis using compound specific reacting tubes. Temperature and
pressure inside the reservoir were monitored using a thermistor, and
a pressure transducer respectively. All the measured parameters
were monitored using a data acquisition system consisting of a 12-bit
16 channel data acquisition board, a terminal board, and computer.
The ore used was ground using a laboratory scale roll mill. Ore
samples were reduced into smaller 1 kg samples by using standard
splitting procedures. The particle size distribution was obtained and is
shown in Table I. In each experiment the column of the reactor was
carefully loaded with 3,000 1 g of the ore. If the ore was to be
loaded with lime, it was previously mixed in small batches. The large
reservoir and smaller reservoirs for electrodes were filled with 1,200
1 ml of the cyanide solution. The solution chemistry was readjusted
depending on the experiment. The electrodes were placed in such a
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1 Copyright 2004 by SME
Preprint 04-64
ON-LINE DIAGNOSTIC OF GOLD LEACHING PARAMETERS
IN A LABORATORY SCALE SIMULATION OF A HEAP LEACH SYSTEM
M. G. Irish
M. J. Jahraus
Anglo Gold North America
Victor, CO
P. R. Taylor
E. E. Vidal
Colorado School of Mines
Golden, CO
way to ensure that no air was left in the smaller reservoirs. The large
reservoir was completely filled with the solution. The peristaltic pump
that circulates the solution through the smaller reservoirs was turned
on at a rate of 30 ml/min. This flow rate ensures that the electrodes
constantly monitor the conditions in the larger reservoir without sig-
nificant delay.
Table I. Particle size distribution of ore used.
Tyler Mesh Retained, %
+4 11.68
-4+6 15.44
-6+12 19.95
-12+32 26.23
-32+150 15.94
-150+325 7.55
-325 3.21
The system was then sealed airtight and the initial parameters
values recorded (pressure, temperature, pH, ORP, [CN
-
], DO).
Previously all the electrodes were calibrated according to recommen-
dations made by the manufacturers. The peristaltic pump that feeds
the solution to the top of the column was calibrated to feed at a rate
of 13.6 ml/min. This flow rate is approximately ten times the typical
flow rates used in gold leaching heaps (0.004 gpm/ft
2
). The experi-
ments were started when the first drop of solution went into the col-
umn. At this point, all the parameters were monitored by the meters
and the data acquisition system at different intervals.
Solution samples were taken from the reservoir for gold, cyanide
and alkalinity determination. Gas samples were also taken to detect
NH3, HCN, O2 and NO2. For free cyanide analysis the standard silver
nitrate method with rhodinine indicator was used; for gold analysis,
atomic absorption (AA) was used.
A total of four experiments are presented using a gold bearing
ore, and adjusted cyanide leaching solutions. Table II shows the
experimental conditions used for this project, while Table III shows the
characteristics of the leaching solutions.
RESULTS AND DISCUSSION
In most of the experiments the ore in the column was complete-
ly wetted by the solution in 30 - 40 minutes. The solution flowed even-
ly through the column without flooding or apparent short-circuiting. In
order to simplify the discussion of results, the experimental results
are presented in two groups: Acid Experiments, and Acid to Basic
Experiments, depending on the variations in pH of the solution.
ACID EXPERIMENTS
Experiments 01 and 02 correspond to tests where no lime was
added to the ore, and hence the re-circulating leach solution was
allowed to become acid. The difference between these two experi-
ments is the initial pH, cyanide and gold concentration. For
Experiment 01, very small amounts of free cyanide and gold were
present, while for Experiment 02 these were increased in order to be
able to detect any changes in their values.
Figures 2 and 3 show plots of the different experimental param-
eters measured in Experiment 01. These graphs are based on vol-
ume of solution cycled through the known amount of ore in column. It
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Figure 1. Schematic drawing of the experimental system.
Table II. Experimental conditions used in this work
Experiment Leaching Solution Ore
01 1,200 ml Solution 00 3,000 g
02 1,200 ml Solution 01 3,000 g
03 450 ml of final Solution from Experiment 02 + 750 ml
of Solution 02 + 50 ml 0.01M NaOH Spent ore from Experiment 02
04 1,150 ml final Solution from Experiment 03 + 12 ml
0.01M NaOH + 30 ml 1M NaOH Spent ore from Experiment 03
Table III. Initial conditions of the leaching solutions used
Solution(a) pH Free Cyanide, ppm Gold, ppm
Solution 00 9.44 1.8 0.4
Solution 01 10.86 150 5.62
Solution 02 11.00 1.8 0.4
Solution 03 11.13 158 5.71
Solution 04 11.03 160 5.79
(a) Solutions 01 through 04 were prepared readjusting the original leaching Solution (00) with additions of NaOH, NaCN and AuCl3 in the required amounts.
is important to note that the concentration of free cyanide is
expressed as a percentage of the initial cyanide concentration meas-
ured by titration.
It can be seen that a sharp decrease in ORP, [CN
-
] and pH are
seen in the early stages of the experiment. It can also be seen that a
slight increase of pressure in the system is observed. The tempera-
ture increased from 22.1 to 23.3C in that interval, possibly indicating
an exothermic reaction.
Two important changes are observed in this experiment, the
drastic change in pH and ORP. The solution had an initial pH value of
9.44 and ORP of +57 mV vs. SHE, which means it was basic and
slightly oxidizing. The lowest value of pH = 4.30 was reached after
only 0.95 ml solution/g of ore went through the column, indicating a
strong acidifying reaction that takes place after the ore comes in con-
tact with the solution. The ORP also becomes strongly negative,
reaching the lowest value of -161 mV vs. SHE after 1.7 ml solution/g
of ore have gone through the column.
There is a pronounced increase in the dissolved oxygen in the
initial phase of the experiment. A peak value of 32.2 mg/l was seen
after one hour and 46 min. of beginning the experiment. No explana-
tion for the appearance of this peak can be given at this point, but
possible causes of the increase are instrumental errors or interfer-
ences from ionic species formed in solution. The dissolved oxygen
levels however returned close to the initial values, after which they
decreased slowly, as expected.
An important increase in pressure is observed in this initial
phase, where the pressure differential with the surrounding atmos-
phere increased up to 27.4 mmHg after only 0.82 ml sol./g ore. The
increase in temperature (1.1C) only accounts for 8% of the total
pressure increase, which means that certain amount of volume of
gases are generated. The total void space in the system for this
experiment was measured to be 1,665 ml. Considering temperature
and barometric pressure corrections, it was calculated that 0.002
moles of gas must have been generated to increase the pressure.
This increase in pressure is likely due to the decomposition of car-
bonates present in the ore due to lower pH values with the subse-
quent generation of CO2. The evolution of CO2 is to be determined in
the next experiments.
After 2.45 ml sol./g ore had passed through the column, gas
samples (300 ml) were taken from the top of the column and 50 ml of
solution was withdrawn from the reservoir. This obviously has an
effect in the pressure of the system, as indicated in the graphs.
Another effect of the sampling is seen where the dissolved oxygen in
solution diminished rapidly right after gas sampling. Hydrogen
cyanide (2 5 ppm) was detected on top of the column, while no NO2
was detected. Oxygen concentration was found to be 21 1 %. At
the end of the experiment gas samples were analyzed as well, but no
NH3, NO2, nor HCN was detected.
The initial free cyanide concentration of the solution used
showed only 1.8 0.4 ppm by titration. This initial value dropped rap-
idly as shown in the graph, but then increased up to 92% of the initial
value. A sample of the solution after 120 hours was titrated giving 0.6
0.4 ppm of free cyanide. Due to the low values of cyanide found in
the initial and final solution, it is not possible to determine exactly the
possible reactions of this free cyanide. It must be mentioned that even
when cyanide was detected in solution during the experiment using
the ion selective electrode, the concentration is too low to consider
the values accurate.
After the initial abrupt changes in the measured parameters in
Experiment 01, most of the values were reaching a steady value near
the conclusion of the experiment. A sharp increase is seen in the
ORP values between 2 and 4 ml sol/g ore in Figure 4. This sharp
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Figure 2. Change of pH, dissolved oxygen and ORP in
Experiment 01.
Figure 3. Change of pressure, temperature and free cyanide
in Experiment 01.
increase was due to an instrumental error that was corrected imme-
diately.
The overall behavior seen is expected in terms of pH, dissolved
oxygen and pressure increase. Two reactions are suspected to be
occurring simultaneously, one is the oxidation of partially oxidized sul-
fide compounds that consume oxygen and acidifies the solution, and
the other is decomposition of carbonates that generates CO2 and
consumes H
+
.
An example of the sulfide reaction that may occur can be with
Fe1-xS:
(1)
At low pH values the calcium carbonate decomposition can be
used as example of an acid consuming reaction:
(2)
These two reactions compete throughout the experiment but ini-
tially the acid forming reaction dominates lowering the pH and dis-
solved oxygen until the sulfide source and available oxygen diminish-
es. Once this initial phase has occurred the carbonate decomposition
dominates, resulting in a slight increase of solution pH and dissolved
oxygen that equilibrates with oxygen from the gas phase.
Other reactions involving the precipitation of Au, and CN con-
sumption must be occurring, but at the concentrations found in this
experiment their effect on the overall behavior is practically nil. It is
suspected that such a strong reduction in the pH and ORP values can
promote the dissociation of the gold complex ion, precipitating the
gold and generating HCN. The reactions would then be:
(3)
(4)
(5)
From gas analysis during the initial phase of the experiment,
HCN was detected in concentration 2 5 ppm.
Gold in the initial, intermediate and final solutions were analyzed
by atomic absorption spectroscopy (AA). The initial Au concentration
in the pregnant solution was only 0.4 0.1 ppm. For solution samples
taken at 8.5, 27.83 and 120 hours, the concentration of Au was about
the same, 0.3 0.1 ppm. Due to the low concentration levels and
error in the AA readings, it is not possible to determine if the gold con-
tent in solution increased or decreased.
Since the values of gold and cyanide concentration were too low
to draw any conclusion, a second experiment was performed, name-
ly Experiment 02. In this experiment the same conditions were used
as in Experiment 01 except for the solution being adjusted with gold
and cyanide additions.
Figure 4 shows the change of pH and gold concentration in solu-
tion to the amount of solution passed through the column. As in
Experiment 01 a sharp decrease in pH is observed in the early
stages. Even when the solution in 02 had a higher pH value (10.86)
compared to the pH of Solution 00 (9.44), it dropped to a minimum of
4.13 which then raised and stabilized to 4.57. Since the initial amount
of gold in solution was high, it is possible to see the change with the
amount of solution passed through the ore. It is clear that the gold
content drops as the solution passes through the column, going from
an initial value of 5.62 ppm down to 5.01 ppm. This reduction in gold
content suggests that at lower pH values, the gold cyanide complex
is no longer stable and the gold could be precipitating from solution
or the ore preg-robbing.
A gas sample was taken after 20 hours of started the experi-
ment (5.5 ml sol./mg ore), and over 400 ppm of HCN was detected.
This high amount of HCN was expected since the solution was
already acid and the cyanide is no longer stable in solution. Other
gases were analyzed, finding no traces of NO2 or NH3. The O2 con-
centration was found to be 20%. By the end of the experiment, the
levels of HCN had dropped down to 280 ppm.
Figure 5 shows the variation of dissolved oxygen, ORP and pH
for Experiment 02. The first conclusion to be drawn is that the peak in
oxygen concentration is product of some chemical properties or reac-
tions that occur during the acidification of the solution, since the same
peak was observed in Experiment 01. This discards any instrumental
error associated with the measurements obtained. As in the previous
experiment, after the peak is reached, the oxygen diminishes, level-
ing off at about 2.02 mg/l. The ORP values are negative and tend to
follow the changes in pH values as before.
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Figure 4. Change of pH and gold content in solution from
Experiment 02 based on volume of solution passed through
the column of ore.
In Figure 6, the changes in pressure, temperature and free
cyanide according to the electrodes is presented. Similar to
Experiment 01, an increase in pressure and temperature suggests
that an exothermic reaction might be taking place and that gases are
being generated. An increase in pressure is likely expected according
to the decomposition reaction of carbonates as explained earlier and
to the generation of HCN gas from the solution.
It was seen that the drop in pH for Experiment 02 was stronger
than that of Experiment 01 despite having a higher initial value. Also
noticeable is the change of dissolved oxygen. It seems that if the pH
of the solution is higher, the dissolved oxygen is lower before the
solution contacts the ore. According to Experiment 01 there is some
oxygen consumption from the solution, while in Experiment 02 this
behavior does not seem to appear.
ACID TO BASIC EXPERIMENTS
In order to determine the effect of increasing the pH of the solu-
tion while the solution is still flowing through the ore, Experiment 03
was performed using the spent ore from Experiment 02 and replac-
ing part of its final solution with Solution 02 (Table III). The experiment
was considered started after 11.98 ml/mg had gone through the
column.
Figure 7 shows the change in pH and gold content of the solu-
tion for this experiment. As before there is a decrease in the pH val-
ues from 12.00 to 5.16 where it stabilized. The gold content in solu-
tion tends to decrease initially from 5.01 to 4.85, but then raises to
5.26. This would seem to indicate a delay in the response of increas-
ing the pH of the solution that at the end seems to re-dissolve
the gold.
Figure 8 on the other hand, shows the change in dissolved oxy-
gen and ORP for this test. Again a peak in dissolved oxygen is seen,
going from an initial value of 6.12 to 18.10 mg/l and decreasing to a
constant value around 5.32 mg/l. The ORP follows the pH tendency,
starting at high positive values and ending in negative figures.
The changes in temperature and pressure for this experiment
are also shown in Figure 9. As in previous experiments there is a rise
in temperature, but in this case a lowering was observed in the pres-
sure. This may suggest that reactions are taking place that consume
compounds from the gas phase, presumably oxygen. The steep
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Figure 5. Change of pH, dissolved oxygen and ORP in solution
from Experiment 02 based on volume of solution passed
through the column of ore.
Figure 6. Changes in pressure, temperature and free cyanide
according to the electrode for Experiment 02 based on volume
of solution passed through the column of ore.
Figure 7. Change of pH and gold content in solution from
Experiment 03 based on volume of solution passed through
the column of ore.
descent seen at around 12.7 ml/mg is due to gas sampling from the
system. As time progressed the pressure started rising again towards
a steady value.
Due to the increase in the gold content observed when the ini-
tial pH was raised in Experiment 03, it was speculated that by con-
stantly increasing the pH of the solution without anymore cyanide
addition might promote the gold levels to rise again. Based on this,
the experiment was continued by first adding 12 ml of 0.01M NaOH
after 18.07 ml/mg had gone through the column. Since no change in
the parameters was detected, it was decided that stronger base solu-
tion should be used.
To start Experiment 04 the system was kept running without
changing solution or ore, and the experiment was considered started
after adding 30 ml of 1M NaOH to the solution. The beginning of this
experiment is at 18.14 ml/mg. During the experiment 10 ml of 1M
NaOH was added every time the pH would drop and stabilize. This
generated peaks in the pH values as shown in Figure 10.
Figure 10 shows that after each peak in pH, the value would
drop back down but to values slightly above the initial reading. As
more solution passed through the column, it is evident that the effect
of adding more NaOH was diminishing the rate of change of the lower
pH readings. The initial drop in pH was 5.30 points, while at the end
of the experiment the drop was only 2.27. During this increase in pH
the gold content in solution rose from 5.19 ppm to 5.68 ppm. It must
be mentioned that these solution tenors were the measured values of
gold corrected for dilutions and sampling done during the experiment.
Figure 11 shows that during the experiment, the dissolved
oxygen was constantly changing during the first part of the test. It can
be seen that during each drop in pH, the dissolved oxygen would
peak. Towards the end of the experiment the changes in dissolved
oxygen practically disappeared stabilizing at 2.88 mg/l. As expected
from previous experiments, the ORP changed in proportion to the
changes in pH. In this case since the final pH was basic (9.57) the
ORP value was positive at 176 mV SHE.
The pressure in the system dropped initially as in Experiment
03, while the temperature rose. This can be seen in Figure 12. The
cyanide electrode also reflects a decrease in free cyanide throughout
the experiment. This suggests that whatever amount of free cyanide
was left from the end of Experiment 03 is being consumed by the sys-
tem since no HCN was detected in the gas phase.
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Figure 8. Change in dissolved oxygen and ORP for solution
from Experiment 03.
Figure 9. Change in pressure, temperature and free
cyanide according to the electrode for solution from
Experiment 03 based on volume of solution passed
through the column of ore.
Figure 10. Change of pH and gold content in solution from
Experiment 04 based on volume of solution passed through
the column of ore.

Combining results from Experiments 02, 03 and 04 gives an
idea of the general tendency of the system when the pH in solution is
allowed to drop to acid conditions and its behavior when the pH is
forced back up into the basic area. Figure 13 shows the pH and gold
concentration changes for the three experiments. It is seen that dur-
ing the drop in pH in Experiment 02, gold was lost from the solution,
but when the pH was increased in Experiment 03 part of the gold lost
was recovered again. As more NaOH was added to the solution in
Experiment 04, the gold content increased to values comparable to
the initial ones found in Experiment 02. This result suggests that the
gold-cyanide complex ion becomes unstable at low pH possibly caus-
ing the gold to precipitate from the solution. Once the pH in the
system rises, the small amount of free cyanide available in solution or
cyanide from other metallic-cyanide complex ion reacts again with the
precipitated gold, recovering it into solution.
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Figure 12. Change in pressure, temperature and free
cyanide according to the electrode for solution from
Experiment 04 based on volume of solution passed
through the column of ore.
Figure 13. Change of pH and gold content in solution from
Experiments 02, 03 and 04 based on volume of solution passed
through the column of ore.
Figure 11. Change in dissolved oxygen and ORP for solution
from Experiment 04.
Figure 14. Change in dissolved oxygen and ORP for solution
from Experiments 02, 03 and 04 based on volume of solution
passed through the column of ore.

Figure 14 shows the change in DO and ORP. Much fluctuation
is observed in these two parameters, but they tend to stabilize once
a higher and stable pH value is obtained. These strong fluctuations
indicate a complex set of oxidation and reduction reactions that occur
during the pH changes. This was evidenced by the formation of pre-
cipitates that were seen in solution.
Fluctuations were also observed in the free cyanide using the
ion selective electrode. Figure 15 shows that during the first phase of
the experiments there is a dramatic decrease in free cyanide levels,
which increase when the first increase in pH was induced starting
Experiment 03. These values then drop and stabilize during
Experiment 04. According to this, cyanide is initially lost to form HCN,
or to form some other cyanide complexes, but then is recovered in
part by raising the pH. As the pH tended to stabilize in the basic
domain, the free cyanide consumption was increasing possibly due to
the dissolution of precipitated gold and re-absorption of HCN from the
gas phase.
During Experiment 03 the solution became acidic and the DO
diminished slightly. During this time the cyanide concentration,
according to the ion selective electrode, also diminished. As expect-
ed the ORP became negative. Results from Experiment 04, on the
other hand, show that the increase in pH to an initial value of 11.38
reduced the measured DO but increased the cyanide concentration
to 27% of the initial solution reading in Experiment 02 as well as the
ORP value. As the solutions pH dropped, remaining basic, the DO
increased and the cyanide reading decreased. This reduction in
cyanide could be only partially attributed to the reaction with precipi-
tated gold from Experiment 02.
In conclusion, from the acid to basic experiments it seems that
gold is lost from the solution when it becomes acid, but can be par-
tially or totally recovered by simply raising the pH again.
CONCLUSIONS AND RECOMMENDATIONS
Several important conclusions and questions have risen from
results obtained from this work. The ore acidifies the leaching solution
when no lime is added to the ore. Oxidation of partially oxidized sul-
fides is the probable cause of the acidifying reaction and increase sul-
fates in solution. Oxygen is consumed from the gas phase when the
pH of the solution is kept basic.
REFERENCES
Bartlett, R.W., 1997, Metal Extraction from Ores by Heap
Leaching, Metallurgical and Materials Transactions B, Vol. 28B, Aug.,
pp. 529-545.
Bouffard, S.C. and Dixon, D.G., 2001, Investigative Study into
the Hydrodynamics of Heap Leaching Processes, Metallurgical and
Materials Transactions B, Vol. 32B, Oct., pp. 763-776.
Kirk, D.W., Foulkes, F.R. and Graydon, W.F., 1978, A Study of
Anodic Dissolution of Gold in Aqueous Alkaline Cyanide, Journal of
the Electrochemical Society, Vol. 125, pp.1436.
Marsden, J., House, I., 1992, The Chemistry of Gold Extraction,
1st ed., Ellis Horwood Ltd.
Sanchez, A.E. and Lapidus, G.T., 1997, Model for heap leach-
ing of gold ores by cyanidation, Hydrometallurgy, Vol. 44, pp. 1-20.
Vorster, B.J., Cyanide Control in the Metallurgical Process of
Gold Extraction in Anglogold (S.A.), Cyanide: Social , Industrial and
Economic Aspects, C. Young, ed., TMS, Warrendale, PA, pp. 535-547.
Wadsworth, M.E., Zhu, X., Thompson, J.S. and Pereira, C.J.,
2000, Gold dissolution and activation in cyanide solution: kinetics
and mechanism, Hydrometallurgy, Vol. 57, pp. 1-11.
Yannopoulos, J.C., 1991, The Extractive Metallurgy of Gold, 1st
ed., Van Nostrand Reinhold, New York, pp.116-120.
SME Annual Meeting
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8 Copyright 2004 by SME
Figure 15. Change in pressure, temperature and free cyanide
according to the electrode for solution from Experiments 02, 03
and 04 based on volume of solution passed through the col-
umn of ore.