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Hydrometallurgy 82 (2006) 118 125 www.elsevier.

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The effect of sulfide minerals on the leaching of gold in aerated cyanide solutions
X. Dai 1 , M.I. Jeffrey ,1
Department of Chemical Engineering, Monash University, Clayton Vic 3800, Australia Available online 8 June 2006

Abstract The effect of galvanic interactions and sulfide mineral dissolution on the gold leaching kinetics in aerated cyanide solutions is investigated. Gold leaching kinetics were measured using a rotating electrochemical quartz crystal microbalance (REQCM), which measures the leaching rates in-situ. When the mineral is electrically in contact with gold, the gold dissolution rate increases as a result of the extra surface area available for oxygen reduction. However the leaching behavior of gold in the presence of soluble sulfide minerals is complicated. It is shown that the formation of sulfide ions in solution results in the passivation of the dissolution of gold. The addition of lead was found to be an effective means of alleviating this problem, as lead promotes the removal of sulfide by precipitation as PbS. 2006 Published by Elsevier B.V.
Keywords: Gold leaching; Kinetics; Cyanidation; Mineral sulfides; Electrochemistry; Passivation; Lead; Galena; Chalcocite

1. Introduction Since a large proportion of gold ores contain sulfide minerals, the effects of these minerals on gold dissolution in cyanide solution have interested many researchers. Early studies on the dissolution of gold in cyanide solution in the presence of sulfide minerals have shown that heavy metal components, such as Cu, Fe and Zn, significantly increase the consumption of both cyanide and oxygen (Habashi, 1967). In addition, the sulfide component has been shown to have a strong impact on the gold leaching kinetics (Fink and Putnam, 1950; Hedley and Tabachnick, 1968). Liu and Yen (1995) conducted a systematic study of the kinetics of gold
Corresponding author. Tel.: +61 8 9334 8081; fax: +61 8 9334 8001. E-mail address: matthew.jeffrey@csiro.au (M.I. Jeffrey). 1 Now at CSIRO Minerals, Bentley, WA, Australia. 0304-386X/$ - see front matter 2006 Published by Elsevier B.V. doi:10.1016/j.hydromet.2006.03.005

dissolution in the presence of various sulfide minerals in both air-saturated and oxygen-enriched systems. Their results demonstrated that the leaching behavior of gold in the presence of sulfide minerals depended strongly on both the solubility of the sulfides and the oxygen concentration in the solution. For instance, in an oxygenenriched cyanide solution, the presence of chalcopyrite, pyrrhotite, arsenopyrite and pyrite were found to increase the gold dissolution rate, while others, such as stibnite and chalcocite, caused a reduction in the gold dissolution rate. Deschenes et al. (2000, 1998), Deschenes and Wallingford (1995) tried to improve the leaching performance of gold in the presence of some sulfide minerals by using pre-leaching, injecting oxygen and adding lead nitrate. It was reported that pre-leaching successfully overcame the effect of pyrite and pyrrhotite on cyanide consumption and the gold leaching kinetics, but it had no beneficial effect when chalcopyrite was present. It was suggested that lead nitrate prevented

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copper and iron dissolution by forming a passive layer at the surface of sulfide minerals. Since the sulfide minerals are to some extent soluble in cyanide solutions, there will always be some sulfur species present in the leaching solution. It is generally believed that the presence of such species results in high consumption of cyanide and oxygen. However, some results of kinetic studies suggest that sulfur species also directly affect the gold leaching reaction. Weichselbaum et al. (1989) found that the addition of trace amounts of sodium sulfide to the cyanide solution dramatically hindered gold leaching and ascribed it to the formation of a passive layer of Au2S on the gold surface. Similar results were obtained by Lorenzen and van Deventer (1992), who studied the kinetics of gold leaching in the presence of reactive sulfide minerals such as pyrrhotite. Jeffrey and Breuer (2000) used gold containing 5% silver rather than high purity gold to investigate the effect of sulfur species and suggested that soluble sulfide hinders the rate of gold leaching by forming a protective layer of the type Au/Sx. They showed that this was a monolayer of sulfur which forms at potentials negative of the bulk sulfur deposition potential. The formation of a monolayer of sulfur on gold in alkaline non-cyanide solutions has also been noted by others (Briceno and Chandler, 1990; Hamilton and Woods, 1983). It was also shown that the sulfur formed is chemically attacked by cyanide, resulting in higher leach rates at higher cyanide concentrations (Jeffrey and Breuer, 2000). Another interesting aspect of the gold leaching behavior is the galvanic interaction between gold and the mineral, as naturally occurring gold is likely to be in contact or in association with various minerals. Lorenzen and van Deventer (1992) tried to differentiate the effect of galvanic interaction from the formation of a passivating film on the gold surface by using pure gold rotating disc electrically contacted with mineral disc in one vessel and then in two separate vessels. They suggested that when gold is in contact with conducting minerals, it will passivate as a result of the enhanced magnitude of the cathodic current. It was argued that the higher cathodic current causes a positive shift in the mixed potential into the passive region, resulting in decreased gold dissolution rates. One complication with most previous studies is that high purity gold was utilized, for which the leaching is hindered by a film of AuCN (Jeffrey and Ritchie, 2001). However most naturally occurring gold contains silver, for which the cyanide leaching reaction occurs at a high rate (Jeffrey and Ritchie, 2000b). The present study aims to establish the effects of sulfide minerals such as

chalcocite on the leaching of gold containing 5% silver using a rotating electrochemical quartz crystal microbalance (REQCM) to directly measure the gold leaching rate and the corresponding mixed potential when it is electrically connected to various mineral sulfide electrodes. 2. Experimental methods These experiments were carried out using solutions prepared from analytical grade reagents and Millipore water. For the experiments without the employment of pre-leaching, cyanide was initially added into the bulk solutions containing sulfide minerals. At different time intervals, sample solutions were taken and filtered, and the filtrate was used to measure gold leach rates using the REQCM, which is described elsewhere (Jeffrey et al., 2000). The concentration of dissolved metal from the sulfides was measured using a Varian SpectrAA-400 Atomic Absorption Spectrometer (AAS). For experiments with pre-leaching, a similar procedure was adopted but cyanide was added after a pre-leaching period of 4 h. The leaching and electrochemical experiments were performed at a rotation rate of 300 rpm and at a temperature of 20 C. All potentials were measured relative to the saturated calomel electrode (+ 0.242 V vs. SHE), but are reported relative to the SHE. Prior to each experiment, gold was electroplated onto the quartz electrode at 25 A m 2 from a solution containing 0.02 mol L 1 potassium dicyanoaurate, 0.23 mol L 1 potassium cyanide, 0.086 mol L 1 potassium carbonate, and 0.5 mmol L 1 silver nitrate. This resulted in a deposit containing approximately 5% silver by mass (which for simplicity will be referred to as gold), thus ensuring that the experiments more closely mimicked industrial conditions. The linear sweep voltammetry was carried out using a PAR273 potentiostat, and a scan rate of 1 mV s 1 was adopted. A platinum wire was used as the counter electrode. 3. Results and discussion 3.1. Electrochemistry of gold and sulfide minerals in cyanide solutions The oxidation of gold and some sulfide minerals in solutions containing 5 mmol L 1 cyanide and 50 mmol L 1 sodium perchlorate as background electrolyte was studied using linear sweep voltammetry, and the polarization curves are shown in Fig. 1. It can be seen that gold oxidation commences at 620 mV and approaches a diffusion limited current of 15 A m 2 at 0 mV. The oxidation of various sulfide minerals was also

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20

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15

i / A m-2

10 Au 5 chalcocite 0 -600 -400 -200 0

gold chalcocite covellite galena pyrite marcasite pyrrhotite chalcopyrite

200

400

E / mV
Fig. 1. Gold and mineral oxidation polarization curves in 5 mmol/L cyanide and 50 mmol/L sodium perchlorate.

studied, and the polarization curves in Fig. 1 show that little current is observed until the potential exceeds 200 mV for pyrrhotite, covellite, pyrite, marcasite, galena and chalcopyrite. The oxidation of chalcocite occurs most readily among the sulfide minerals studied, with the reaction commencing at 150 mV. However, it is still much more noble than gold in cyanide solutions. These results demonstrate that gold cannot be cathodically protected by these minerals when in electrical contact. In a similar manner, the polarization curves for the reduction of oxygen in the absence of cyanide on the mineral surface were obtained (Fig. 2). It is clear that oxygen reduction occurs on all the minerals, with chalcocite having the most active surface for reduction, and galena the least active surface. Since the oxidation of gold can occur at potentials more positive than 600 mV, it is clear from Fig. 2 that there is the opportunity for galvanic interaction between the gold and sulfide minerals. It can be expected that particularly for chalcocite, oxygen reduction on the mineral surface in contact with gold will give rise to higher dissolution rates. 3.2. Effect of galvanic interactions on gold leaching In order to study the galvanic interactions between sulfide minerals and gold in more detail, two electrodes, one gold electrode and one mineral electrode, were simultaneously leached in 5 mmol L 1 cyanide solution. The REQCM was used to measure the gold leaching rate and the corresponding mixed potential when it was electrically connected to a chalcocite electrode. The two electrodes were not connected together electrically until leaching had proceeded for 5 min. As shown in Fig. 3, it is clear that the mass of gold decreases at a steady rate prior to the electrical connection of the mineral. From the slope of mass vs. time, the gold leaching rate is calcula-

ted to be 5.6 10 5 mol m 2 s 1 under these conditions. This leaching rate is typical for the dissolution of gold in air saturated solutions when the rate is oxygen diffusion controlled (Jeffrey and Ritchie, 2000b), and hence it represents the maximum rate at which gold can be leached in air saturated cyanide solutions. After the gold and chalcocite electrodes were electrically connected together, the gold leaching rate increased, reaching a value of 13 10 5 mol m 2 s 1. At the same time the mixed potential increased rapidly from 350 to 60 mV, before slowly decreasing to 200 mV. As shown in Fig. 2, this is in the potential region where oxygen reduction can occur on the mineral surface. Therefore, it is believed that the connected mineral electrode provides extra surface area for oxygen reduction to occur, and hence the increase in the total cathodic current causes a positive shift in the mixed potential and an increase in the gold leaching rate. A similar effect was observed for the other sulfide minerals, even galena, for which oxygen reduction is more difficult. However the increase in leaching rate when galena was connected was less significant than for chalcocite. It is worth noting that these results are inconsistent with those of Lorenzen and van Deventer (1992), as they stated that the enhanced cathodic current shifts the mixed potential to the passivation region for gold, and hence hinders the dissolution process. It is most likely that this difference can be ascribed to the fact that Lorenzen and van Deventer (1992) used a pure gold electrode, for which the leaching is hindered (Jeffrey and Ritchie, 2001). As shown in Fig. 1, the gold/silver alloy does not experience passivation, and hence an increase in the mixed potential gives rise to higher leaching rates. The second mechanism by which sulfide minerals can impact on the gold leaching process is as a result of their
0

-2

i / A m-2

-4
Chalcocite Galena Pyrite Marcasite Pyrrhotite Chalcopyrite

-6

-8

-10 -600

-400

-200

E / mV
Fig. 2. Oxygen reduction polarization curves on various sulfide minerals in 5 mmol/L cyanide and 50 mmol/L sodium perchlorate.

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0 0 -100 -200 -300 -150 -400 -200 0 200 400 600

121

-50

-100

t/s
Fig. 3. Effect of the galvanic interaction between gold and chalcocite on the leaching of gold and on the mixed potential in 5 mmol/L cyanide.

solubility. The experiments shown in Fig. 3 were only run for a short period of time, and hence the nonoxidative dissolution of the sulfide minerals was limited. Since most sulfide minerals are to some extent soluble in cyanide solution, it has been suggested that the dissolved species may affect the gold leaching reaction. The remainder of the present study will address this issue. 3.3. Effect of galena (PbS) on gold leaching kinetics The REQCM was used to study the leaching of gold in air saturated 10 mmol L 1 cyanide solutions in the presence of galena (PbS). At various time intervals a sample of solution was filtered and the gold leaching rate was determined by measuring the mass as a function of time using the REQCM. The steady state leach rate was then calculated and found to remain constant above 6 10 5 mol m 2 s 1 for three hours. It is worth noting that the concentration of lead measured in the solution for the experiments was less than 5 ppm. However with time, the colour of the solids changed from black to a milky white. Such a result suggests that in cyanide solutions, the galena is converted to lead hydroxide via the oxidation of the sulfide. Previous studies have shown that lead catalyses the oxidation of soluble sulfide to thiocyanate through the precipitation of lead sulfide (Hedley and Tabachnick, 1968; Jeffrey and Breuer, 2000). Thus it is believed that galena is oxidized to thiocyanate, producing lead ions which precipitate to form the milky white lead hydroxide. 3.4. Effect of pyrite (FeS2), pyrrhotite (Fe1xS) and marcasite (FeS2) on gold leaching rates Using the same method as described above for galena, gold leaching experiments were performed to study the effect of pyrite, pyrrhotite and marcasite. Fig. 4

shows the gold dissolution rates as well as the iron concentrations as a function of contact time of the solution with 1 g/L of mineral. It can be seen that the solubility of these three minerals in cyanide solution is very low with less than 2 mg/L iron detected after three hours of leaching. Surprisingly, pyrite appeared to be more reactive than the other two iron mineral samples. The gold leaching rate was also measured as a function of time, but due to the low solubility of the minerals, the gold dissolution rate is barely affected by the presence of these minerals (Fig. 4). A leaching rate of ca. 5.5 10 5 mol m 2 s 1 was observed for pyrrhotite and macarsite. However it is interesting to note that for pyrite, the gold leaching rates, ca. 4.5 10 5 mol m 2 s 1 are slightly lower than that for the other two minerals. Such a result is consistent with the apparent higher reactivity of pyrite than marcasite and pyrrhotite. The non-oxidative dissolution of the mineral produces a low concentration of dissolved sulfide, which is well known to passivate gold leaching in cyanide solutions (Fink and Putnam, 1950; Hedley and Tabachnick, 1968; Weichselbaum et al., 1989; Jeffrey and Breuer, 2000). 3.5. Effect of the copper cyanides on the gold leaching rate One of the complications with studying the leaching of gold in the presence of copper sulfides is that there is the possibility of low free cyanide concentration due to the formation of copper cyanide species 2 such as Cu(CN)3 . Thus preliminary experiments were carried where cuprous oxide was added to the cyanide solution, and the copper concentration and gold leaching
2.0

m /g

E / mV

[Fe] / ppm 105 r / mol m-2s-1

1.5 1.0 0.5 0.0 6 4 2 0 0.0


pyrite pyrrhotite marcasite

0.5

1.0

1.5

2.0

2.5

3.0

t / hr
Fig. 4. The iron concentration (top) and gold leaching rate (bottom) as a function of the contact time for solutions containing 10 mmol/L cyanide and 1 g/L sulfide minerals.

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5 4 3 2 1 0 0 1 2 3 0 1

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4.4 280

105 r / mol m-2 s-1

3.6 3.2 2.8 2.4 2 3

[Cu] / ppm

10mM CN12mM CN13.5mM CN-

cyanide:copper ratio

4.0

240 200 160 120 80 40 0 0.0 0.5 1.0 1.5 2.0


without lead 10ppm lead 20ppm lead 100ppm lead

t / hr
Fig. 5. The gold leaching rate (left) and cyanide to copper ratio (right) as a function of the contact time for solutions containing 2 mmol/L Cu2O and various cyanide concentrations.

2.5

3.0

t / hr
Fig. 6. The effect of lead addition on the copper concentration vs. time profile for solutions containing 13.5 mmol/L cyanide and 2.4 g/L chalcocite.

105 r / mol m-2 s-1

rate were measured as a function of time. The results in Fig. 5 show that Cu2O dissolved rapidly in the cyanide solution, forming soluble copper cyanide complexes as reflected in the low cyanide to copper ratio. For the solution initially containing 10 mmol L 1 cyanide, it is clear from Fig. 5 that the cyanide to copper ratio is below 3. Hence the dominant species in the solution would be 2 Cu(CN)2 and Cu(CN)3 . In contrast, when the solution contained 13.5 mmol L 1 cyanide, the cyanide to copper ratio is well over 3, and hence the solution would contain free cyanide. The effect of the copper to cyanide ratio on the gold leaching rate is shown in Fig. 5. It is clear that the gold leaching rate remains at ca. 4.5 10 5 mol m 2 s 1 as long as there is sufficient free cyanide in solution. At the cyanide to copper ratio of approximately 3, where most 2 of the copper cyanide is present as Cu(CN)3 , reasonable 5 2 1 gold leaching rates of ca. 1.5 10 mol m s can still be achieved. However, when the cyanide to copper ratio drops to 2.5 and a large proportion of copper is present as Cu(CN)2 , the gold leaching rates are extremely low. This 2 suggests that Cu(CN)3 has a reasonable capability of leaching gold according to Eq. (1), while Cu(CN)2 cannot. This conclusion is consistent with other researchers' work (Jeffrey et al., 2002; Muir et al., 1991; Parsons et al., 1993; Zheng et al., 1995).
4Au 8CuCN2 3 O2 2H2 O4AuCN2 8CuCN 2 4OH

cyanide solutions; with 140 mg/L copper being observed after 10 min, and 230 mg/L after 1 h. The high solubility obviously poses a problem in cyanidation, as copper cyanide complexes consume free cyanide and reduce the gold leaching rate. In addition, the presence of dissolved sulfide ions is known to be detrimental to the leaching of gold. Thus experiments were performed to establish whether the addition of 10, 20 or 100 mg/L lead could reduce the solubility of the chalcocite. Fig. 6 shows that the addition of 10 or 20 mg/L has little effect, whilst 100 mg/L lead does reduce the dissolution of chalcocite with only 200 mg/L copper detected after 3 h. Despite this, a reasonable quantity of sulfide would be leached into the solution. The gold leaching rate was then measured in solutions that had been in contact with chalcocite for various times up to 3 h (Fig. 7). It can be seen that the presence of chalcocite in cyanide solution after 0.25 h dramatically

5 4 3 2 1 0 0.0 0.5 1.0 1.5 2.0 2.5 3.0


without lead 10ppm lead 20ppm lead 100ppm lead

3.6. Effect of chalcocite (Cu2S) on gold leaching rates The gold leaching rate and the dissolved copper concentration were measured for different contact time of the cyanide solution with chalcocite. The results plotted in Fig. 6 show that chalcocite dissolves rapidly in

t / hr
Fig. 7. The effect of lead addition on the leaching rate for gold in air saturated 13.5 mmol/L cyanide solutions after contact with 2.4 g/L chalcocite for various time intervals.

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8
20 ppm lead No lead

123

105 r / mol m-2 s-1

5 4 3 2 1

No galena with galena

i / A m-2

0 -600

-500

-400

-300

-200

-100

0 0.0

0.5

1.0

1.5

2.0

2.5

3.0

E / mV (SHE)
Fig. 8. Polarization curves showing the effect of lead addition on the gold oxidation half reaction in 13.5 mmol/L cyanide solutions after contact with chalcocite for 3 h.

t / hr
Fig. 9. The effect of 200 mg/L galena addition on the leaching rate of gold in 13.5 mmol/L cyanide solutions after contact with 2.4 g/L chalcocite for various time intervals.

retards gold dissolution in the absence of lead, and where 10 mg/L lead was added. In the past it has been argued that such an effect is due to the consumption of cyanide. However, from the data in Fig. 6, the amount of copper dissolved is only 140 mg/L and one would expect sufficient free cyanide to leach the gold readily. Fig. 7 also shows that when 20 mg/L lead was added, the gold leaching rate is substantially faster. These results indicate that some other factor apart from cyanide consumption is responsible for the adverse effect of chalcocite on gold leaching, and this effect can be alleviated by lead addition. It has been previously proposed that a passive film of sulfur formed on the surface of gold may be responsible for the reduced gold leaching rates in sulfide containing solutions (Jeffrey and Breuer, 2000). If this is the case, then the role of the added lead is to prevent the passive film from forming. This has been observed for synthetic solutions containing lead nitrate and sodium sulfide (Jeffrey and Breuer, 2000). It is worth noting that when 100 mg/L lead was added, although the gold leaching rate was high initially, after 1 h or more of contact between the solution and mineral, the leaching rate shown in Fig. 7 is severely hindered. Such a result suggests that the addition of too much lead can be detrimental to the gold leaching process, and it has been suggested in the past that overuse of lead could result in the passivation of the gold surface, presumably by lead hydroxide (Habashi, 1970). The effect of lead on the gold oxidation half reaction was studied using standard electrochemical techniques. Fig. 8 shows the comparison of the polarization curves in the solutions with and without lead after being in contact with chalcocite for 3 h. It is clear that the oxidation of gold is active in the solution containing lead, whereas it is passive in the absence of lead. This result is consistent with the above conclusions. The peak appearing in the

polarization curve of the solution containing lead is related to the formation and decomposition of a metallic lead or goldlead alloy film (Deschenes et al., 2000; Jeffrey and Ritchie, 2000a). Further experiments were conducted to investigate the addition of galena as a source of lead for improving the dissolution of gold in cyanide solutions in the presence of chalcocite. This was accomplished by adding 200 mg/L galena into the bulk solution containing chalcocite. The results shown in Fig. 9 without galena addition are the same as that shown in Fig. 7. After 10 min the gold leaching rate in the presence of galena and chalcocite is still low due to the slow dissolution of galena. However after 1 h of leaching in the presence of chalcocite, it is clear that the gold leaching rate is significantly enhanced by the presence of galena in the bulk solution cf. Fig. 7 with 20 mg/L lead added into the bulk solution. The polarization curve of gold oxidation in the solution that had been contacted
50 40
No mineral Chalcocite + 20 ppm lead Covellite + 20 ppm lead Chalcocite Covellite Galena

[Au] / ppm

30 20 10 0 0 1 2 3 4

t / hr
Fig. 10. The effect of lead addition on gold dissolution in a solution containing 10 mmol/L cyanide, about 50 mg/L pure gold powder and various sulfide minerals.

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with galena and chalcocite for 3 h was also similar to that when 20 mg/L lead was added as lead nitrate. 3.7. Gold powder leaching in the presence of various sulfide minerals The experimental results shown above illustrate the effect of galvanic interactions and mineral dissolution on gold leaching separately. In order to study galvanic interactions and mineral dissolution together, gold powder leaching experiments were carried out in the presence of ground sulfide minerals. The limitation of these experiments is that a pure gold powder was used, as compared to a gold/silver alloy in the other leaching experiments. However, as shown in Fig. 10, the data obtained from this experiment is very informative. In the absence of minerals, the gold leaching rate was relatively slow, with a gold concentration of 35 ppm being obtained in 4 h (equivalent to 70% gold dissolution). In the presence of galena, the leaching of gold was much more rapid, consistent with the above discussion. In the case where either chalcocite or covellite was present, the gold leaches very slowly. After 4 h, only 15% gold was leached in the presence of chalcocite, and only 7% gold in the presence of covellite. After 24 h, the amount of gold extracted was 59% and 36% in the presence of chalcocite and covellite, respectively. These results are consistent with a passive film formed on the surface of gold when soluble sulfide is present in the solution. Experiments performed with the addition of 20 mg/L lead as lead nitrate to the cyanide solutions containing chalcocite or covellite show much more rapid gold leaching (Fig. 10) verifying the experiments carried out using the REQCM. 4. Conclusions For gold leaching in the presence of sulfide minerals, there are two major mechanisms by which the sulfide can impact on the gold leaching rate (a) through the galvanic interaction between gold and the conducting mineral in contact with gold and (b) through the dissolution of the mineral which impacts on the solution speciation. An electrochemical study of the oxidation of gold and sulfide minerals in the cyanide solutions shows that none of the mineral studied, including chalcocite, covellite, galena, pyrite, pyrrhotite, marcasite and chalcopyrite, are oxidized at more negative potentials than gold, and thus do not cathodically protect the gold when in direct contact with the mineral. Oxygen reduction occurs at different rates on the sulfide mineral surfaces, and hence when the gold is in contact with the mineral, the higher

cathodic current shifts the mixed potential more positively, resulting in a higher dissolution rate. The leaching behavior of gold in the presence of sulfide minerals is quite complicated due to the dissolution of the mineral to form sulfide in the solution that then impacts on the gold leaching kinetics. It has been shown that gold leaching in cyanide solutions is severely hindered by the presence of chalcocite due to the high solubility of this mineral in cyanide solutions. The gold leaching rate in solutions containing chalcocite can be improved by the addition of 20 mg/L lead during the cyanide process. The role of lead is to promote the precipitation of PbS and enhance the anodic oxidation of gold via a goldlead alloy film. The addition of galena to the cyanide solution containing chalcocite was shown to have the same effect as the addition of lead nitrate. References
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