Hydrometallurgy 108 (2011) 109114

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Hydrometallurgy
j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / h yd r o m e t

Implementation of sodium hydroxide pretreatment for refractory antimonial gold

and silver ores
Oktay Celep a, brahim Alp a,, Doan Paktun b, Yves Thibault b
a
b

Mining Engineering Department, Karadeniz Technical University, 61080, Trabzon, Turkey

CANMET Mining and Mineral Sciences Laboratories, 555 Booth Street, Ottawa, Ontario, Canada

a r t i c l e

i n f o

Article history:
Received 14 January 2011
Received in revised form 11 March 2011
Accepted 13 March 2011
Available online 3 April 2011
Keywords:
Gold
Silver
Cyanidation
Antimony
Refractory ore
Alkaline leaching

a b s t r a c t
Alkaline pretreatment of a refractory goldsilver ore containing antimony minerals such as stibnite, andorite
(Sb3PbAgS6) and zinkenite (Pb9Sb22S42) was tested using sodium hydroxide in order to determine its
effectiveness in improving the recovery of gold and silver. Mineralogical investigations show that silver was
present as andorite and Au/Ag alloy. Gold particles have been observed as associated with quartz and
inclusions within the antimony minerals. Increasing the sodium hydroxide concentrations from 0.5 to 5 mol/L,
increasing the temperature from 20 to 80 C, and reducing the particle size from 50 to 5 m enhanced the
removal of antimony from the ore. Up to about 75.5% Sb removal was achieved by alkaline pretreatment, which
in turn remarkably improved the extraction of silver from levels of less than 18.7% to 90% and gold from less
than 49.3% to 85.4% during subsequent cyanidation. These ndings, consistent with mineralogical results,
suggest that alkaline leaching can effectively be used as chemical pretreatment method as an alternate to the
alkaline sulde leaching in the processing of refractory antimonial goldsilver ores.
2011 Elsevier B.V. All rights reserved.

1. Introduction
The Akoluk ore deposit, hosted by volcanicsedimentary rocks of
the Eastern Pontides, is situated near Ordu in northeastern Turkey.
The ore deposit contains a variety of sulde and oxide minerals, as
well as native gold (Tysz and Akay, 2000; Yaylal-Abanuz and
Tysz, 2010). Total reserves are estimated to be about 1 million
tonnes (Anon, 1993). The most signicant trace and minor minerals
are associated with stibnite and zinkenite (PbSb sulfosalt), which
along with sphalerite are the most widespread ore minerals in the
deposit (Ciftci, 2000). According to Aslaner and Ottemann (1972),
gold occurs as inclusions in zinkenite (PbSb2S4). Recently, Celep et al.
(2009) reported that the ore consisted predominantly of quartz, the
illite/kaolinite group of clay minerals and barite with lesser amounts
of pyrite, stibnite, sphalerite, zinkenite and andorite. Gold occurs as
small particles ranging from 1 to 88 m in association with sulde
minerals and quartz. Cyanide leaching tests of 24-h duration showed
that metal extractions were consistently low, at less than 47% for
gold and less than 19.2% for silver. Diagnostic leaching tests suggested
that the decomposition of the sulde could improve the extraction
of gold and silver by about 29.5% and 56.7%, respectively. Detailed
mineralogical characterization of the Akoluk goldsilver ore has
indicated that the ore contains antimony suldes, including andorite
(Sb3PbAgS6) and zinkenite (Pb9Sb22S42), as the main silver and gold

Corresponding author. Fax: + 90 4623257405.

E-mail address: ialp@ktu.edu.tr (. Alp).
0304-386X/$ see front matter 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.hydromet.2011.03.005

carriers (Alp et al., 2010; Celep et al., 2011). Ultrane grinding and
roasting of the ore were ineffective as pretreatment for improving
the recovery of gold and silver by cyanidation (Celep et al., 2010).
Cyanidation tests also showed that lead nitrate addition had a limited
effect on gold and silver extractions. The low gold and silver
extractions from the ore indicated its refractory nature to cyanide
leaching and the need for a suitable chemical pretreatment process to
improve metal dissolution.
Refractory gold ores do not respond to direct cyanidation;
therefore, such ores have to be pretreated prior to cyanidation to
liberate the contained gold and silver so that they are readily
amenable to extraction (La Brooy et al., 1994). Roasting, pressure
oxidation, bio-oxidation and, to a limited extent, ultrane grinding
have been commercially applied to increase gold recoveries from
refractory ores (Corrans and Angove, 1991; Iglesias and Carranza,
1994; Gunyanga et al., 1999). Alkaline sulde leaching is a suitable
pretreatment process for antimonial ores and concentrates (Ubaldini
et al., 2000; Bal and Achimoviov, 2006; Curreli et al., 2009; Awe
and Sandstrm, 2010; Awe et al., 2010) by making the silver available
to cyanide solutions or removing the hazardous or penalty elements
such as As and Sb from the ores and concentrates. Alp et al. (2010) and
Celep et al. (2011) have already shown that alkaline sulde leaching
is an effective pretreatment method ahead of cyanide leaching for
the extraction of gold and silver from antimonial refractory ores.
Recoveries as high as 90% Ag and 82.6% Au were achieved after
the removal of 95% Sb in an alkaline pre-treatment stage under the
conditions of 4 mol/L Na2S and NaOH, 15 m particle size, and 80 C
(Alp et al., 2010). In addition, increasing NaOH concentrations

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O. Celep et al. / Hydrometallurgy 108 (2011) 109114

enhanced the dissolution of Sb-bearing minerals. This nding was

consistent with reports on leaching of antimonial suldes such as
stibnite (Anderson and Krys, 1993; Ubaldini et al., 2000; Sminckov
and Komorov, 2005; Sminckov, 2009). Sminckov (2009)
showed that the leaching of stibnite by sodium hydroxide was
possible. Bal (2000) showed that proustite (Ag3AsS3) and pyrargrite
(Ag3SbS3) decompose during the alkaline leach, which makes
high silver recovery possible during subsequent cyanidation. No
such studies on alkaline pretreatment of antimonial ores containing
andorite (Sb3PbAgS6) and zinkenite as the main gold/silver bearing
minerals have been reported in the literature.
Recent studies (Alp et al., 2010, Celep et al., 2011) indicated that
gold losses (up to 13%) occur during the alkaline sulde leaching
and the losses increase at high temperatures and high concentrations of sulde. Furthermore, considering the problematic health
issues associated with the sulde leaching, this study was designed to
evaluate alkaline leaching using sodium hydroxide as a potential
pretreatment process alternative to alkaline sulde leaching.
2. Experimental
2.1. Materials
The ore used in this study is an antimony-rich refractory gold
silver ore from Akoluk (Ordu-Turkey). The ore samples were reduced
in size by crushing and grinding. A laboratory-scale stirred media mill
was used for ne grinding (80% passing size, d80 = 50, 15 and 5 m)
prior to the leaching tests. Particle size analysis of the ore samples was
performed by a Malvern Mastersizer 2000 model laser analyzer.
The earlier chemical and mineralogical studies (Celep et al., 2009)
indicated that it is a high grade gold and silver ore assaying at 220 g/t
Ag and 20 g/t Au. In addition, the ore contained 52.2% SiO2, 17.1% Ba,
4.7% Al2O3, 6.9% S, 1.6% Sb, 1.5% Zn, 1.3% Fe2O3, 0.4% Pb, 0.02% As
and 0.04% Cu (all in weight percent). Quartz, the illite/kaolinite
group clay minerals and barite are the predominant phases in the ore.
Pyrite, stibnite, sphalerite, zinkenite and andorite are the main sulde
minerals identied in the ore (Celep et al., 2011).

Cyanide leaching of the residues was then carried out to determine the effects of alkaline leaching pretreatment on the extraction
of gold and silver. Glass reactors (1 L) were used for cyanide leaching
of the residues. The reactors were mechanically agitated with
pitched-blade turbine impellers and aerated at a ow rate of 0.3 L/
min (Alp et al., 2010; Celep et al., 2011). NaCN (Merck) and NaOH
were used to adjust the pH at 10.5 during cyanidation. In all tests,
10-mL samples were taken from the leach pulp at pre-determined
time intervals and then centrifuged to obtain clear aliquots for the
determination of Au, Ag and free cyanide in solution. Silver nitrate
titration in the presence of p-dimethylamino-benzal-rhodanine
(0.02% w/w in acetone) as the indicator was used to determine
the concentration of free CN in samples (Celep et al., 2011). If
required, concentrated cyanide solution (5% NaCN) was added to
maintain free CN concentration at the initial level of 1.5 g/L NaCN,
and consumption of NaCN was recorded (Celep et al., 2011). On the
termination of cyanide leaching tests, the residues were digested
in acid (HCl, HNO3, HClO4 and HF) to determine the undissolved
metal content. Analysis of gold, silver and antimony from the solutions was carried out using an atomic absorption spectrometer (AASPerkin Elmer AAnalyst 400). The extraction of metals was calculated
based on the metal content of leaching residues.
3. Results and discussion
3.1. Alkali pretreatment
Alkaline leaching has a signicant advantage over the alkaline
sulde leaching due to lower reagent costs. In addition, a small amount
of gold can be dissolved in alkaline sulde solutions (Anderson, 2001;
Jeffrey and Anderson, 2003; Alp et al., 2010; Celep et al., 2011). This
situation will bring additional costs in the course of gold recovery
from solution. The alkaline sulde leaching has also potential environmental issues related to the formation of H2S gasses.

2.3. Experimental work

3.1.1. Dissolution of metals during pretreatment

Alkali pretreatment of the ore at 15 m (d80 particle size) using
3 mol/L NaOH at 80 C in sodium hydroxide solution caused the
dissolution of elements in the following proportions: 64.4% Sb, 0.5%
Ag, 0.06% Fe, 1.5% Cu, 0.05% Zn and 0.03% Pb. The pretreatment had no
effect on the dissolution of gold. The results indicate that sodium
hydroxide leaching is highly selective for the removal of antimony
from the ore.
Although alkaline leaching using alkali metal hydroxides is
potentially applicable to elements that form anionic complexes such
as Al, Sb, As, Cu, Fe and Pb, the higher metal extractions would require
high pressure or temperatures under oxidizing conditions (Gupta and
Mukherjee, 1990; Filippou et al., 2007). The alkaline leaching (3 mol/L
NaOH, 80 C, d80: 15 m) had no important effect on the dissolution
of metals with the exception of antimony. For this reason, the effects
on the removal of antimony of NaOH concentration, temperature
and particle size were investigated.

Tests were designed to evaluate the effects of sodium hydroxide

concentrations, temperature and particle size (d80: 550 m). The
ground samples (d80: 50 m) were leached in a 1-L glass reactor
immersed in a water bath to control the leaching temperature (20
80 C) within 2 C. The vessel with 200-mL leach solution (NaOH)
and 70 g ore sample (solids 35% w/vol) was continuously stirred
at 750 rpm. Sodium hydroxide (NaOH, assay 99.9% Merck) in the
range of 0.55 mol/L NaOH was used to maintain the alkalinity. The
leach solution was sampled (10 mL) at regular time intervals for
the analysis of antimony. At the end of leaching after 120 min, solid
and liquid phases were separated by ltration and the ltrates
were analyzed for Sb, Au, Ag, Pb, Zn, Cu and Fe. The residues were airdried, and sampled for analysis to determine the metal recoveries.

3.1.2. Effect of NaOH concentration

The effect of leaching time on antimony removal from the ore was
investigated at different reagent concentrations (0.55 mol/L NaOH)
at the xed slurry temperature of 80 C. The experimental results are
presented in Fig. 1. Antimony dissolution varies between 10.4 and
70.1%. Increasing leaching time resulted in the increase of antimony
extraction. Most of antimony dissolution had occurred within the
rst 5 min at high reagent concentrations. When the leaching time
was increased to 2 h, antimony removal was improved only slightly,
even at 5 mol/L NaOH.
Fig. 1 shows the effect of NaOH concentration (0.55 mol/L) on
the removal of Sb from the ore (d80 = 15 m) at 35% w/v solids
and 80 C. The dissolution of Sb improved with increasing the

2.2. Mineralogical characterization of the ore

Mineralogical analysis of the ore sample was performed to determine gold and silver bearing phases. Characterization studies were
carried out using a FEI Quanta 400MK2 Scanning electron microscopy
(SEM) equipped with EDAX Genesis 4XMI at the Mineral Research
and Exploration Institute of Turkey and a HITACHI variable-pressure
SEM with a Link microanalysis system at CANMET. Microanalysis of
the mineral grains was performed by a JEOL JXA 8900 electron
probe X-ray microanalyzer (EPMA) at CANMET utilizing ve wavelength dispersive spectrometers (WDS) operated at 20 kV with a
probe current of 20 to 30 nA.

O. Celep et al. / Hydrometallurgy 108 (2011) 109114

100

100

0.5 M NaOH
1 M NaOH
3 M NaOH
5 M NaOH

20C
40C
60C
80C

80

Sb removal, %

80

Sb removal, %

111

60

40

60

40

20
20
0
0

0
0

20

40

60

80

100

20

120

40

60

80

100

120

Leach time, min.

Leach time, min.

Fig. 1. Effect of leaching time and NaOH concentrations on the removal of antimony
from the ore (d80: 15 m, 80 C).

concentration of NaOH. The highest removal of Sb at 70.1% was

achieved at the highest reagent concentration of 5 mol/L NaOH. The
benecial effect of sodium hydroxide pretreatment is attributed to the
decomposition of antimonial phases such as andorite, stibnite and
zinkenite present in the ore. Based on the speciation of Sb (Fig. 2),
decomposition of these phases by hydroxide would release antimony

in the form of species such as SbO

2 , Sb(OH)4 , Sb(OH)6 , SbOS , and
SbS
(Bal,
2000;
Anon,
2005).
Sminckov
(2009)
reported
that
2
stibnite was dissolved as SbOS and SbS
2 species (Eq. (1)) in the
leaching by sodium hydroxide (at 0.54 wt.% NaOH). In the case of the
arsenical silver-bearing sulde minerals such as proustite (Ag3AsS3)
in alkaline leaching, it was indicated that silver could remain in Ag2S

Fig. 3. Effect of leaching time and temperature on the removal of antimony from the ore
(3 mol/L NaOH, d80: 15 m).

(Eq. (2)) phase which is highly soluble within cyanide solutions

(Bal, 2000). It is afrmed that the antimonial minerals such as
andorite and zinkenite as well as stibnite can be decomposed with
similar mechanism.

Sb2 S3s + 2NaOH NaSbOSaq + NaSbS2aq + H2 O

2Ag3 AsS3s + 6NaOH3Ag2 Ss + Na3 AsO3aq + Na3 AsS3aq + 3H2 O

2
3.1.3. Effect of temperature
The inuence of temperature (2080 C) on the release of antimony
during the NaOH alkaline pretreatment (3 mol/L NaOH, d80: 15 m
and 120 min.) is shown in Fig. 3. An increase of temperature from 20
to 80 C improved the antimony extraction. At 20 C, only 23.1% of
the antimony was solubilized from the ore. The extraction of Sb was
substantially improved to 64.4% with an increase in the temperature

100

Sb removal, %

80

60

40
50 m
15 m

20

5 m
0
0

20

40

60

80

100

120

Leach time; min.

Fig. 2. EhpH diagrams of the system SbOH (Sb = 10 10 mol/L, 25.15 C, 105 Pa.)
(JNC-TDB/GWB) (Anon, 2005).

Fig. 4. Effect of particle size on the removal of antimony from the ore (3 mol/L NaOH,
80 C).

112

O. Celep et al. / Hydrometallurgy 108 (2011) 109114

a 100

Ag extraction, %

80

60
as-received ore
after alkaline leach

40

20

0
0

12

16

20

24

Leach time, hours

Fig. 5. Au particle in quartz matrix with framboidal pyrite.

b 100
to 80 C. These ndings suggest that temperature is the most inuential
factor in the alkaline treatment process.

Ag recovery, %

3.1.4. Effect of particle size

The effect of particle size of the ore (d80: 51550 m) on the
alkaline leaching process was studied at a xed reagent concentration
of 3 mol/L NaOH, and a slurry temperature of 80 C. Decreasing the
particle size (d80) from 50 to 5 m produced a positive effect on the
solubilization of Sb, which improved from 54 to 72.5% Sb removal
(Fig. 4). In addition to increased surface area and liberation of
antimony suldes, the benecial effect of reducing particle size can be
also attributed to mechanical activation phenomena as reported by
Bal (2000).
It appears that not all the antimony is responding to alkaline
leaching. Approximately ~25% antimony remained in the residue. It
appears that the framboidal pyrite with concentric enrichments of
antimony and silver is probably responsible for this behavior (Fig. 5,
Table 1). In this case, unrecovered antimony would represent the
amount tied to framboidal pyrite.

R = 0.9775

80

60

40

20

0
0

20

40

60

80

100

Sb removal, %
Fig. 6. (a) Effect of pretreatment on the silver extraction by cyanidation (3 mol/L NaOH,
80 C, d80: 5 m) and (b) dependence of the cyanide extraction of silver on the removal
of antimony by the alkaline pretreatment (d80: 15 m, 80 C).

3.2. Cyanidation after treatment

The inuence of the sodium hydroxide alkaline pretreatment
prior to cyanidation was shown to be effective for the decomposition
of the most of antimony minerals. All cyanidation tests indicated
that silver and gold recoveries improved after antimony removal

Table 1
Microprobe phase analyses from spots in Fig. 5.
Spot

wt.%

Gold

Pyrite

Pyrite

Pyrite

Pyrite

Au
Ag
Cu
Fe
Sb
Pb
As
Zn
S
Si
O
Total

85.57
13.79

3.63
0.32
33.77
8.32
5.38
0.62
0.08
44.5
0.09
2.91
99.62

0.18
0.36
42.23
1.76
0.58
0.69
0.31
49.09
0.06
2.07
97.33

0.78
0.41
41.16
1.67
1.21
0.57
0.14
48.85
0.26
2.16
97.21

0.25
0.34
42.01
1.77
0.78
0.58
0.55
48.81
0.05
2.94
98.06

99.36

by alkaline leach. While less than 18.7% Ag was extracted from the
untreated ore, 90% of the silver was recovered following 75.5%
antimony removal by alkaline leaching (Fig. 6). The highest silver
recovery (90% Ag) was obtained with 3 mol/L NaOH at 80 C and
5 m particle size. Similarly, gold extraction was shown to improve
from 49.3% to 55.885.4% following the pretreatment (Fig. 7). The
high overall Au and Ag extractions with pretreatment conrm that
a large proportion of the gold and silver was refractory in nature
because of their occurrence in the structures or as unliberated
(i.e. locked) inclusions in the antimony minerals that are apparently
insoluble in cyanide solutions.
The occurrence and association of gold and silver are illustrated
in Fig. 8 where sections of the feed sample were analyzed under
SEM-WDS. Table 2 shows the results of microprobe analyses of the
phases within the numbered spots in Fig. 8. Andorite is the main
gold and silver-bearing mineral in the ore (Fig. 8). Gold particles
containing silver also occurred associated with quartz and as inclusions within the minerals such as andorite (Table 2). Andorite were
identied to be the most important Ag bearing sulde phase. These
ndings indicate andorite (Sb3PbAgS6) and zinkenite (Pb9Sb22S42) as
the main gold and silver bearing and hosting minerals (Celep et al.
2011) are not amenable to cyanide leaching without NaOH pretreatment process.

O. Celep et al. / Hydrometallurgy 108 (2011) 109114

113

100

Au extraction, %

80

60

40

as-received ore
after alkaline leach

20

0
0

12

16

20

24

Leach time, hours

b 100
80

Au recovery, %

R = 0.9457
60

40

20

0
0

20

40

60

80

100

Sb removal, %
Fig. 7. (a) Effect of pretreatment on the gold extraction by cyanidation (3 mol/L NaOH,
80 C, d80: 5 m) and (b) dependence of the cyanide extraction of gold on the removal
of antimony by the alkaline pretreatment (d80: 15 m, 80 C).

Fig. 8. Backscattered electron images showing the locations of microprobe analyses

listed in Table 2. (a) Disseminated gold grains (white) and SbPbAg sulde
(whitish gray) in andorite grains (light gray) (b) SbAg sulde grains (white) in
quartz (gray).

The consumption of cyanide was determined to be 4.85 kg NaCN

per ton of the ore. In comparison with the consumption of 9.1 kg/t
for the untreated ore (Celep et al., 2009), this gure represents a
signicant reduction in cyanide consumption with important cost and
environmental implications, including the treatment costs of residual
cyanide in the tailings pond water. Thus, the alkaline pretreatment
process is considered to be an appropriate method for processing
of the antimonial refractory goldsilver ores.

recoveries reached 90% from very low levels of 510%. A signicant

increment in gold and silver extractions corresponded to the
removal of antimony from the ore during the alkaline pretreatment.
Based on mineralogical investigation, silver was present as andorite
and Au/Ag alloy. Gold particles containing silver have been
observed as associated with quartz and inclusions within the
antimony minerals such as andorite. These ndings were consistent
with the alkali pretreatment results. Experimental results demonstrated that sodium hydroxide pretreatment is a viable extractive
metallurgy technique for the processing of refractory antimonial
gold and silver ores. Mineralogical characterization of materials
resulting from alkaline pre-treatments could shed further light on
mechanisms of Au and Ag liberation and will be discussed in details
at another paper.

4. Conclusion
Sodium hydroxide pretreatment of the refractory goldsilver
ore from the Akoluk deposit showed that up to 75.5% of the
antimony can be removed by adjusting the molar concentration of
the leaching solution. Temperature, particle size and NaOH
concentrations were identied to be the most important factors
affecting the extraction of antimony and subsequent cyanide
extraction of silver and gold. Whereas the direct cyanidation
resulted in gold recoveries of about 49.3%, the alkaline pretreatment process signicantly improved the gold recovery to 85.4%.
With the removal of about 75.5% Sb during pretreatment, Ag

Acknowledgements
Sincere thanks and appreciation go to the General Directorate of
the Mineral Research and Exploration of Turkey (MTA) for SEM-EDX
analysis and to Anatolia Minerals Development Ltd. for kindly
providing the ore samples.

114

O. Celep et al. / Hydrometallurgy 108 (2011) 109114

Table 2
Microprobe analyses (wt.%) of andorite, an unknown SbAg sulde, gold and quartz grains shown in Fig. 8.
Spot

10

wt.%

SbPbAg sulde

Andorite

Andorite

Andorite

Gold

Gold

Gold

SbAg sulde

SbAg sulde

Quartz

6.7
0.3
32.9
38.3
20.2

10.1
1.3
40.3
26.0
21.8

84.8
14.6
0

88.2
11.9
b 0.1

85.5
12.7
b 0.1

12.7

13.1

51.7

52.2

34.2

34.3

Au
Ag
Cu
Sb
Pb
S
Si
O
Total

98.4

99.5

11.4
1.5
42.8
22.0
22.4

100.1

9.9
1.4
40.8
25.9
21.9

99.9

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