Int. J. Miner. Process.

82 (2007) 178 – 186

www.elsevier.com/locate/ijminpro

Leaching of an oxide gold ore with chloride/hypochlorite solutions

Morteza Baghalha ⁎
Department of Chemical and Petroleum Engineering, Sharif University of Technology, Azadi St., Tehran, 11365, Iran
Received 3 April 2006; received in revised form 25 July 2006; accepted 6 September 2006
Available online 17 October 2006

Abstract

An oxide gold ore was subjected to chloride/hypochlorite leaching at room temperature. The effects of three factors, including
Ca(OCl)2 vs. NaOCl, OCl− concentration, and HCl concentration on gold leaching performance were investigated. Due to
formation of CaOCl+ complex in solution and hence less reactivity, calcium hypochlorite produces a sluggish gold leaching
kinetics, taking twice the time (46 h) to achieve maximum gold recovery of 58% compared to sodium hypochlorite. 10 g/L of total
initial hypochlorite species in solution produces reasonable gold recoveries. The amount of added HCl and hence the initial pH was
found to have a major effect on gold leaching kinetics and maximum gold recovery. A high level of 9 g/L of added HCl causes
HClO to be very reactive, producing very fast kinetics, reaching 67% gold extraction in 4 h. It also causes a faster consumption of
hypochlorous acid, through catalytic decomposition (by NiO and CuO) and disproportionation. Hypochlorous acid reactions with
sulfide and ferrous content of ore proceed very slowly in the pH range of 4–11. Gold–chloro complexes are strongly adsorbed on
quartz component of ore. To minimize this undesirable adsorption of gold–chloro species, the aging time must be limited to a few
hours only.
© 2006 Elsevier B.V. All rights reserved.

Keywords: Chloride; Hypochlorite; Hypochlorous; Lixiviant; Gold; Ore; Leaching; Adsorption; Gold–chloro; Complex

1. Introduction One of the strongest oxidizing agents for this system is

chlorine. As Reaction (1) shows, chlorine, in presence of
Chlorine had been used to dissolve gold from ores chloride ions, readily dissolves elemental gold to gold
and concentrates, during the second half of the 19th (III)–chloro complex, [AuCl4]−, provided the pH is less
century in Australia and North America. At the begin- than 2 (Finkelstein et al., 1966).
ning of the 20th century, this process was gradually
replaced by the more economical alkaline cyanide 2Au þ 3Cl2 þ 2Cl− →2½AuCl4 − ð1Þ
leaching (Sparrow and Woodcock, 1995). Nowadays, The rate of dissolution of gold by chlorine is much
however, due to the realization of environmental prob- faster than that by cyanide (Filmer et al., 1984). Also, due
lems of cyanide, there is a worldwide quest to find to presence of chloride ions, there is no passivation of gold
viable alternatives to cyanide. One of the alternatives is surfaces during chlorination. The major disadvantage of
a chloride solution with an appropriate oxidizing agent. the chlorine–chloride system is the high reactivity of
chlorine in reaction with sulfide and gangue carbonate
⁎ Tel.: +98 21 6616 5465; fax: +98 21 6602 2853. minerals. As a result, only high grade materials may be
E-mail address: [email protected]. treated by chlorine–chloride system economically.
0301-7516/$ - see front matter © 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.minpro.2006.09.001
 M. Baghalha / Int. J. Miner. Process. 82 (2007) 178–186 179

Another widely used oxidizing agent for gold– After pressure oxidation of the concentrate and sub-
chloride system is hypochlorite. Jeffrey et al. (2001a,b) sequent hypochlorite leaching, the recoveries increased
recently measured the dissolution rate of pure gold and an to 90% for gold and 93% for silver. In contrary to
Au/Ag alloy in chloride/hypochlorite solutions using a reducing ores and concentrates, some ores may naturally
rotating electrochemical quartz crystal microbalance. contain oxidizing agents, such as MnO2. Gold in these
They showed that at pH = 8 where hypochlorite ion types of materials can be leached with an NaCl/acid
(ClO−) is the dominant oxy-chloride species, the dis- solution only. Since the oxidant Cl2/HClO is formed in-
solution rate of the gold disk was very low. However, at situ upon reaction of Cl− and MnO2 (Leon and Quispe,
more acidic pHs, hypochlorous acid forms according to 1986), for in-situ chlorine/hypochlorous acid formation,
Reaction (2). MnO2 have been used in NaCl and H2SO4 solution to
leach gold from anode slimes (Hait et al., 2002).
Hþ þ ClO →HClO ð2Þ Another complexity in gold–chloride system is strong
adsorption of gold–chloro complexes on mineral sur-
HClO is a stronger oxidizing agent than ClO−, hence faces, such as goethite, quartz, and alumina (Machfsky
leaches gold faster (Jeffrey et al., 2001a,b). Reaction (2) et al., 1991). Gold(III)–chloride adsorption by goethite
has an equilibrium constant of 107.5 at 25 °C (Snoeyink (FeOOH) was specifically investigated by Machfsky et al.
and Jenkins, 1980); hence, at pH = 7.5, concentrations of (1991) as a function of pH (4 to 8) and Cl− concentrations
ClO− and HClO are equal. For pHs lower than 7.5, (0 to 0.1 M). In 0.1 M NaCl solution and pH = 4, gold
HClO becomes the dominant species. adsorption on goethite was 4000 ppm. The adsorption
At 1.0 M NaCl concentration and potentials higher increased as pH increased from 4 to 7. This trend is
than 950 mV (vs. SHE), AuCl4− species is the stable opposite to typical behavior for anion adsorption onto
gold–chloride complex in solution up to pH = 10 (Wang, oxide surfaces. This “retrograde” adsorption trend is due
1992). Leaching of gold with hypochlorous acid follows to a shift in dominance from AuCl4− at pH = 4 to adsorbed
Reaction (3). hydroxyl-substituted species (such as AuCl(OH)3−) at
higher pH values (Machfsky et al., 1991). Based on gold
2Au þ 3HClO þ 5Cl þ 3Hþ →2½AuCl4  þ 3H2 O and iron Mossbauer spectroscopy, it has been confirmed
ð3Þ that gold–hydroxo–chloro complexes are strongly
adsorbed by iron oxides such as goethite (Greffie et al.,
The mechanism of gold dissolution in chloride solu- 1996). Based on Mossbauer spectroscopy technique,
tions involves the initial formation of Au(I)–chloride adsorption of AuCl4− on modified activated carbons was
complex (AuCl) on the surface of metallic gold. AuCl also studied in an aging process through a course of
undergoes further complexation with chloride ion to several weeks (Cashion and Brown, 1998). It was shown
AuCl2−. This complex then moves to solution and is that adsorption on the solid surface first results in the loss
oxidized with HClO to AuCl4−(Nicol, 1980; Nikoloski, of one of the chloride ions. Subsequent reduction of Au3+
1998). to Au+ results in the loss of two more chloride ions.
Based on weight loss of gold strips, Tran et al. (1992, Finally the last chloride ion may be removed and gold
2001) measured gold dissolution rate in different precipitates as Au0. The following species were identified
chloride/hypochlorite mixtures. For instance, with a on the solid surfaces: AuCl4−, AuCl3X−, AuCl2X2−,
concentration of 100 g/L NaCl and 10 g/L OCl− at 20 °C AuCl2− , and AuClX− , where X is an oxygen- or
and pH = 6.0, gold dissolution rate was measured at nitrogen-containing group. To avoid the complexity of
13 mg/cm2 h. This rate is much higher than the gold gold species adsorption and precipitation, some research-
dissolution rate of 2.5 mg/cm2 h obtained in 2 g/L of ers have opted to measure gold leaching kinetics in
cyanide solution (Tran et al., 2001). idealized chloride/hypochlorite system in terms of weight
The performance of chloride/hypochlorite solution loss of pure gold disk and strips, rather than measuring
for gold leaching also depends on major minerals pres- dissolved gold concentration in solution (Jeffrey et al.,
ent in the ore. Gold–chloride complex is rather unstable 2001a,b; Nikoloski, 1998).
and may re-precipitate upon contact with a reductant, The objective of this work was to examine the
such as sulfidic materials of ore. Puvvada and Murthy viability of using chloride/hypochlorite lixiviant sys-
(2000) used chloride/hypochlorite solution to leach gold tem to leach gold from an oxide gold ore. Further-
and silver from a chalcopyrite concentrate. Direct hypo- more, due to the possibility of using heap leaching
chlorite leaching of the sulfidic concentrate yielded gold technique for this deposit, tests were designed to run
and silver recoveries of 43% and 45%, respectively. in the absence of oxygen. This condition mimics the
180 M. Baghalha / Int. J. Miner. Process. 82 (2007) 178–186

Fig. 2. XRD analysis of an oxide gold ore. A: ankerite, Ca(Fe,Mg)

(CO3)2; M: muscovite, H2KAl3(SiO4)3; Q: quartz, SiO2.

dip tube and another to the top of slurry. To ensure that

the reactor pressure does not exceed 10 psig during
overnight operation, a suitable relief valve was con-
Fig. 1. Experimental setup for chloride/hypochlorite leaching of a gold nected to the second nitrogen gas port. Leaching tests
ore, under 5 psig nitrogen pressure. were run at room temperature (24 ± 1 °C).
Before starting a test, pH, ORP, and DO probes were
case of a compact heap, where air can hardly pene- calibrated. 2 kg of ground ore feed was poured to the
trate into the heap. reactor. 4 kg of tap water was added to the reactor and
agitation was set at 600 rpm. Solid NaCl was then
2. Experimental added. To de-oxygenate the reactor, nitrogen gas was
bubbled into the slurry through the dip tube. It normally
A 4 in. core from an oxide gold deposit was crushed took about 30 min for the DO probe to show a zero value
and ground to an average size of 150 μm. It was then reading for dissolved oxygen in slurry. After this period,
passed through a Knelson gravity concentrator to sepa- nitrogen gas injection was switched from the dip tube to
rate its coarse gold nuggets. The concentrator tailing the other port. The required amounts of reactive re-
was used for leaching tests. Commercial grade reagents, agents, e.g., 36% HCl solution, and 5% NaOCl solution,
including 36% HCl, 5% NaOCl, solid NaCl, and solid were poured into the reactor. Tap water was then added
Ca(OCl)2 were used for the tests. Tap water with a TDS to obtain 6 kg of total solution in the reactor (a solid to
(total dissolved solids) of less than 50 ppm was used. liquid ratio of 0.33 was maintained for all tests). pH,
Leaching tests were performed in a custom-made 10 l ORP, DO, and temperature readings were recorded
Plexiglas stirred tank vessel. A simple drawing of the immediately (at t = 0 h). After each data collection, the
setup is shown in Fig. 1. A turbine-type Teflon impeller electrodes were taken out, washed and stored. The main
was used for agitation. A large port on the lid was port was closed and nitrogen pressure was allowed to
assigned for the feed introduction and sampling. This build up to set point pressure of 5 psig (by using a gas
port was also used for entrance of pH, ORP, DO, and regulator).
temperature probes. As shown in Fig. 1, two smaller The tests were run for up to 5 days. In day one,
ports were used for nitrogen gas injection, one through a electrode readings and samples were collected at 0.25, 1,

Table 1
Major elements composition (wt.%) of the gold ore
SiO2 Na K Mg Ca Al Fe (total) Fe (ferrous) C (total) C (inorganic) S (total) S (sulfide)
54.4 0.7 1.3 4.3 4.4 5.8 4.9 4.4 3.1 2.9 0.5 0.5
 M. Baghalha / Int. J. Miner. Process. 82 (2007) 178–186 181

Table 2 allowed to settle for 5 min. 20 mL supernatant clear

Experimental conditions for the chloride/hypochlorite leaching tests solution sample was collected by a syringe. The sample
Test no. Solid/liquid ratio Oxidant OCl− Cl− HCl (36%) was filtered through a 0.2 μm syringe filter and stored
(S/L) type (g/L) (g/L) (g/L) for later solution analyses. Agitation was restarted, the
1 0.33 Na(OCl) 10 61 3.3 main port was closed and the test was continued. For
2 0.33 Ca(OCl)2 10 61 3.3 finishing the test, nitrogen gas was closed and slurry was
3 0.33 Ca(OCl)2 2.7 61 3.3
filtered in a pressure filter using air at 20 psig pressure.
4 0.33 Na(OCl) 10 61 9
5 0.33 Na(OCl) 10 61 0 The filter cake was twice washed with 2 kg tap water
and dried in an oven at 80 °C overnight. After drying,
the solid residue was pulverized and sent for gold fire
2, 3, 4, 5, and 6 h. For the following days, data and assay analysis. The solution samples were also analyzed
samples were collected once per day. To perform data for gold by fire assay method. Concentration of hypo-
collection and sampling, the reactor pressure was re- chlorite ion in a solution sample was measured based on
leased through a valve. The main port was then opened. a standard titration method using thiosulfate solution
To inhibit oxygen penetration to the reactor, nitrogen (Clesceri et al., 1998).
was allowed to sweep through the reactor on top of
slurry and exit from the main port continuously. The 3. Results
electrodes were inserted into slurry. After waiting for
2 min for stable electrode readings, the values were Due to coarse nature of gold in the ground ore (the
recorded and electrodes were taken out. For sample Knelson tailing), gold head assay for each leaching test
collection, agitator was turned off. The solids were was calculated by adding gold remained in solid residue

Fig. 3. Chloride/hypochlorite leaching. Temperature = 25 °C, solid/liquid (S/L) ratio = 0.33, Cl− = 61 g/L. The performance of Ca(OCl)2 vs. Na(OCl).
182 M. Baghalha / Int. J. Miner. Process. 82 (2007) 178–186

and the gold leached. The calculated gold content was in these tests are shown in Fig. 3. Fig. 3A shows that percent
the range of 1–2 g/t. The analyses of major elements of leached gold peaked at 58% and then dropped in both
ore, obtained by flux fusion-ICP technique, are reported cases. In test #1 for NaOCl, the peak occurs at 23 h, and in
in Table 1. An XRD analysis of the ground ore was test #2 for Ca(OCl)2, it occurs at 46 h. In Fig. 3B,
performed to obtain its mineralogical characterization. hypochlorite ion concentration in solution vs. time is
As shown in Fig. 2, the major minerals identified were: shown. Fig. 3C shows that the initial pH for both tests was
ankerite, Ca(Fe,Mg)(CO3)2 (A); muscovite, H2KAl3 8. The solution pH dropped to a value between 5.5 and 6
(SiO4)3 (M); and quartz, SiO2 (Q). Three minor phases in about 23 h, and then increased. The solution redox
may also exist (very small peaks not marked in Fig. 2). potential is shown in Fig. 3D. By comparing Fig. 3B
These are: albite, (Na, Ca)Al(Si,Al)3O8; diaspore, and D, it is understood that as long as small amounts of
Al2O3.H2O; and chlorite, (Mg,Fe)5(Al,Si)5O10(OH)8. OCl− exists in solution, redox potential remains higher
Five gold leaching tests were performed for up to than 1000 mV (vs. SHE). When all hypochlorous acid is
5 days. The experimental conditions of these tests are consumed, redox potential drops below 1000 mV and
reported in Table 2. The solid to liquid ratio for all tests gold starts to drop out of solution either through precipi-
was set at 0.33. The concentration of NaCl for all tests was tation to metallic gold or through adsorption on mineral
set at 100 g/L, equivalent to 61 g/L of Cl− ion. Three other surfaces (Fig. 3A). From the results of tests #1 and #2, it is
factors, including oxidant type, concentration of OCl−, seen that Ca(OCl)2 and NaOCl behave rather similarly,
and concentration of HCl varied among tests. In tests #1 except that maximum leached gold for Ca(OCl)2 occurs at
and #2, two oxidizing agents, Ca(OCl)2 and NaOCl, were a longer time (Fig. 3A). This may be due to formation of
compared. The initial concentration of OCl− = 10 g/L and Ca(OCl)+ complex in solution. The formation of this
HCl = 3.3 g/L were the same for both tests. The results of complex, in turn, reduces concentration of HClO in

Fig. 4. Chloride/hypochlorite leaching. Temperature = 25 °C, solid/liquid (S/L) ratio = 0.33, Cl− = 61 g/L. Effect of OCl− concentration on gold
leaching behavior of the ore.
 M. Baghalha / Int. J. Miner. Process. 82 (2007) 178–186 183

solution, which results in slower gold leaching kinetics The effect of initial acidity on gold leaching perfor-
(refer to Reaction (3)). mance was studied at three levels of added HCl. The
The effect of initial concentration of oxidizing agent results of these three tests at 9, 3.3, and 0 g/L of added
on gold leaching performance was investigated at two HCl (tests #4, 1, and 5, respectively) are shown in Fig. 5.
concentrations of OCl−, 10 and 2.7 g/L. The results of The best performance of gold leaching, in terms of fast
these tests (#2 and #3) are presented in Fig. 4. As kinetics and maximum recovery, occurs at 9 g/L of
shown in Fig. 4A, maximum dissolved gold in solution added HCl, i.e., test #4 in Fig. 5A. As shown in Fig. 5C
was 58% and 24% for the high and low values of and B for test #5 with 0 g/L HCl, the initial pH equals 11
OCl−, respectively. As depicted in Fig. 4C, the initial and OCl− reactivity and its initial consumption are low.
pH for test #2 at 10 g/L OCl− is higher than that for The low reactivity of OCl− causes very slow kinetics for
test #3 with 2.7 g/L OCl−. According to Reaction (2), gold leaching, Fig. 5A. On the other extreme, when 9 g/
this is due to higher consumption of H+ for test #2 L HCl was added in test #4, the initial pH was 7.3, and
with higher OCl−. However, after 10 h, the solution pH very fast gold leaching kinetics was achieved, i.e., 67%
for test #2 becomes more acidic. Obviously, the higher in 4 h. However, as shown in Fig. 5B, initial
level of HClO have caused acid-producing reactions consumption of OCl− in this test was very high, i.e.,
(as discussed later) to proceed faster. In conclusion, the 63% in 0.25 h. In summary, at least 9 g/L of HCl must be
initial concentration of OCl− must be at least 10 g/L to used to achieve fast and high gold recoveries. Among
achieve high gold leaching values for the tested ore. the three factors tested in this study, initial solution pH

Fig. 5. Chloride/hypochlorite leaching. Temperature = 25 °C, solid/liquid (S/L) ratio = 0.33, Cl− = 61 g/L. Effect of HCl concentration on gold leaching
behavior of the ore.
184 M. Baghalha / Int. J. Miner. Process. 82 (2007) 178–186

has the most profound effect on gold leaching in

hypochlorite/chloride system. One of the effects of pH is
on the distribution of solution species. Using HSC
Chemistry software (Outokumpu Research, Pori, Fin-
land), Eh–pH diagram of chloride/hypochlorite system
at 25 °C (for total Cl concentration of 2 M) was
constructed (Fig. 6). A similar diagram (for total
Cl = 1e − 4 M) is also given elsewhere (Snoeyink and
Jenkins, 1980). The total Cl concentration only affects the
Cl2-dominant region for very acidic pHs. Fig. 6 shows
that for pH values less than 7.5 and redox potentials
higher than 1200 mV, the dominant species is HClO.
According to Reaction (3), high concentrations of HClO
and H+ causes a very high extraction rate of gold, as
evidenced in test #4, Fig. 5A.
Two of the leach residues (#1 and #4) were selected Fig. 7. Percent Ca and Mg leached from ankerite during test #1. Based
for elemental and XRD analyses. The obtained results on simple mass balance calculations, ankerite in the ore has the
showed virtually no differences with those of ore feed, composition Ca(Fe0.71, Mg0.29)(CO3)2. Weight percentage of this
in terms of sulfide, ferrous, and ankerite content. compound in the ore is estimated to be roughly 23%.
Hence, it is concluded that these compounds would
react very slowly with hypochlorite solutions at the calculations showed an Fe/Ca molar ratio of 0.71.
pHs investigated in this study. To verify this further, Charge neutrality of ankerite also dictated an Mg/Ca
two solution samples from test #1 were analyzed for molar ratio of 0.29. Therefore, ankerite in the feed is
dissolved metals by ICP. The only significant elements estimated to have the composition Ca(Fe0.71, Mg0.29)
found were Mg and Ca with concentrations in the (CO3)2, with a weight percentage of roughly 23%.
range of 150 to 700 ppm. Among the identified major Ankerite reacts slowly in hypochlorite/chloride solu-
minerals of ore (Fig. 2), ankerite is the only mineral tion and produces the dissolved Ca2+ and Mg2+ species
that contains inorganic carbon and calcium. Based on in solution. Based on the measured concentrations of
values in Table 1, molar ratio of C/Ca in ore feed is 2.2 Ca2+ and Mg2+, percentage of ankerite leached was
which is close to the theoretical value of 2 in ankerite. calculated, as shown in Fig. 7 (leached values are
Ferrous iron also exists only in ankerite. Mass balance consistent for both Ca and Mg). This figure shows that
less than 6% of ankerite has been leached; hence, it re-
confirms the low reactivity of ankerite in the
experimental range of this study.

4. Discussion

It is estimated that only a few percentage of ferrous

iron and sulfide content of ore feed react with hypo-
chlorite solution in pH range of 4 to 11. Hypochlorous
acid is reduced to chloride ion (Reaction (4)); sulfide-
containing components are oxidized and produce sulfate
ions (Reaction (5)); and ferrous iron is oxidized to ferric
iron (Reaction (6)).

HClO þ Hþ þ 2e →Cl þ H2 O ð4Þ

þ 
ð1=4ÞS2 þ H2 O→ð1=4ÞSO2
4 þ 2H þ 2e ð5Þ

2FeO þ H2 O→Fe2 O3 þ 2Hþ þ 2e ð6Þ

Fig. 6. Eh–pH diagram of chloride/hypochlorite system at 25 °C. Total
Cl concentration = 2 M. This diagram was produced with HSC In addition to Reaction (4) that consumes hypochlor-
Chemistry software (Outokumpu Research, Pori, Finland). ous acid due to reaction with sulfide and ferrous iron,
 M. Baghalha / Int. J. Miner. Process. 82 (2007) 178–186 185

hypochlorous acid may also disproportionate chemical- 5. Conclusions

ly to chlorate ion, Reaction (7) (Currey and Pumplin,
1988). It may also undergo a decomposition reaction, Chloride/hypochlorite lixiviant system at room
Reaction (8). This reaction is catalyzed by mineral temperature was used to leach gold from an oxide
surfaces, such as NiO and CuO (Vogt et al., 1986), that gold ore. To find the optimal operating conditions, the
are present in the feed at 400 and 150 ppm, respectively. effect of three factors, including Ca(OCl)2 vs. NaOCl,
OCl− concentration, and HCl concentration were in-
ClO þ 2HClO→ClO 
3 þ 2Cl þ 2H
þ
ð7Þ vestigated. Calcium hypochlorite produced a sluggish
gold leaching kinetics, requiring twice more time (46 h)
2ClO →2Cl þ O2 ð8Þ
to achieve the maximum gold recovery of 58%
For all tests, except #3 (with low initial OCl−), solu- compared to sodium hypochlorite. To have a reasonable
tion pH initially drops, reaches a minimum, and then gold leaching kinetics, it was found that OCl− in solu-
slightly increases. The initial pH drop must be due to net tion must be equal or higher than 10 g/L. The amount of
acid generation in Reactions (4)–(7). These are pre- HCl added and hence initial pH was found to have a
dominant reactions when hypochlorous acid concentra- major impact on gold leaching kinetics and maximum
tion is relatively high. When it decreases sufficiently, gold recovery. A very slow gold leaching kinetics was
acid in solution is slowly neutralized with alkali com- obtained when no acid was added. On the other extreme,
ponents of ore. 9 g/L of added HCl caused a very high reactivity that
It is shown in Figs. 3B, 4B, and 5B that depending produced a very fast gold leaching kinetics. Hypochlo-
on solution pH, a large proportion of hypochlorite rite species reactions with sulfide and ferrous content of
content of solution disappears in 0.25 h. If this large ore were found to be insignificant in the pH range of 4 to
drop in ClO− concentration were due to Reactions 11. Adsorption of gold–chloro complexes is anticipated
(4)–(7), the solution pH would have reduced to very to occur on quartz minerals in our system. To minimize
low levels, and virtually all sulfide and ankerite of ore adsorption of gold–chloro complexes, it works best to
feed would have reacted. On the other hand, if the minimize the aging time.
drop were due to Reaction (8), catalyzed on NiO and
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