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A Review on the Recovery of Noble Metals from Anode Slimes

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A Review on the Recovery of Noble Metals from

Anode Slimes

Wei Dong Xing, Seong Ho Sohn & Man Seung Lee

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the Recovery of Noble Metals from Anode Slimes, Mineral Processing and Extractive Metallurgy
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MINERAL PROCESSING AND EXTRACTIVE METALLURGY REVIEW
https://doi.org/10.1080/08827508.2019.1575211

A Review on the Recovery of Noble Metals from Anode Slimes

Wei Dong Xinga, Seong Ho Sohnb, and Man Seung Leea
a
Department of Advanced Materials Science & Engineering, Institute of Rare Metal, Mokpo National University, Chonnam, Korea; bIncheon
Technology Service Centre, Korea Institute of Industrial Technology, Songdo-dong, Incheon, Korea

ABSTRACT KEYWORDS
Anode slimes resulting from the electrorefining of Cu, Pb, Sn, and Zn contain noble metals, such as Au, Anode slimes; noble metals;
Ag, and platinum group metals. Pretreatments have been employed to enrich the noble metals by pretreatment; leaching;
removing base metals from the anode slimes. The enriched residues are dissolved in diverse aqueous separation
systems such as cyanide, thiosulfate, thiourea, and halide in the presence/absence of oxidizing agents.
Separation of noble metals from the solution depends on the nature of the leaching solutions. Solvent
extraction, ion exchange, electrowinning, and some novel technologies are employed for the separation.
The advantages and disadvantages of each separation process were reviewed. Moreover, new materials
for the separation of noble metals have been introduced.

1. Introduction adequate aqueous solution and then the noble metal ions in
the leaching solutions are separated by employing solvent
Anode slimes result from the electrorefining of metals such as
extraction and ion exchange. In this review, the pretreatment
copper, lead, tin, and other metals. Noble metals like gold,
methods are classified according to the chemical composition
silver, and platinum group metals (PGMs) are present in these
of metals in anode slimes. The characteristics and perfor-
anode slimes. Among these anode slimes, the weight percen-
mance of several kinds of leaching agents were reviewed.
tage of the noble metals is the highest in the copper anode
Separation of the noble metals in the leaching solution was
slime. The average concentration of gold in the anode slimes
summarized together with the recently developed novel
is about 40 ppm and the total amount of anode slimes pro-
separation technologies.
duced annually in the world are almost 55,000 t/year (Green
2006; Hait et al. 2009; Safarzadeh et al. 2018). These noble
metals are widely employed in the manufacture of advanced 2. Pretreatment of anode slimes
materials and thus anode slimes attract much attention as
During the electrorefining of metals, parts of base metals and
valuable resources containing the noble metals (Butterman
impurities report to the anode slimes. Therefore, in order to
1988; Chen and Dutrizac 1990, 1993; Wang et al. 2014;
improve leaching and separation efficiency, the anode slimes
Shibata 2015). In general, noble metals exist as either alloys
are pretreated by some methods depending on the composi-
with other base metals or metallic compounds in the second-
tion of anode slimes. These methods can be classified into
ary resources. Table 1 lists the weight percentage and the
three categories, namely pyrometallurgy, hydrometallurgy,
nature of noble metals in several types of anode slime,
and combination of pyro and hydrometallurgy. High pressure
which affects the processes for the recovery of valuable com-
(Chen and Huang 2006; Dorfling 2012), vacuum (Lin and Qiu
ponents present in anode slimes (Donmez et al. 1998; Hou
2011, 2012; Qiu et al. 2012), microwave (Al-Harahsheh and
2000).
Kingman 2004; Tokkan et al. 2012; Ma et al. 2015), ultrasound
Much research has been done on the recovery of noble
power (Şayan and Bayramoğlu 2004; Öncel et al. 2005; Chang
metals from diverse anode slimes. In anode slimes, the base
et al. 2017) are employed in the pretreatments to improve the
metals generally cover the surface of the anode slimes or form
process efficiency.
metallic compounds with noble metals (see Table 1).
Moreover, noble metals exist as their oxidized states in sele-
nides, tellurides, and sulfides. Therefore, oxidation of the 2.1. Copper anode slimes
anions is needed to liberate the noble metal ions. Alloys
Based on the mineralogical characterization of copper anode
usually demand a higher oxidizing potential than their pure
slimes in Table 1, the base metals including Te, Sb, Se, and As
metal components. Therefore, the base metals should be
form metallic compounds with noble metals. These metallic
removed prior to the recovery of noble metals. Afterwards,
compounds strongly influence the recovery of gold and silver
the concentrates containing noble metals are dissolved into an
together with other PGMs. Depending on the weight

CONTACT Man Seung Lee mslee@mokpo.ac.kr Department of Advanced Materials Science & Engineering, Institute of Rare Metal, Mokpo National
University Chonnam, Chonnam 534-729, Korea
Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/gmpr.
© 2019 Taylor & Francis Group, LLC
2 W. D. XING ET AL.

Table 1. The main compounds and composition of noble metals in different anode slimes.
Anode slime Contents Compounds of precious metals Resource
Copper anode slimes 1–28% Ag, 0.1–1.5% Au, ~70g/t Ag2Se, Ag2Te, CuAgSe, Au2Te, AgAuTe; a (Hou 2000)
PGMs. little of AgCl
1.2% Au, 20% Ag. (Ag, Au, Cu)2(Se, Te), AgCl The Balkhash GMK (Antipov and Tarasov 2002)
Au < 0.1–0.12% AuTe, Ag, Ag3Sb, (Cu, Ag)2OSeO2 The Kovoguty Krompakhi Plant (Antipov and Tarasov
2002)
1.54% Ag, 0.1% Au Ag2Se Indian Copper Complex (Hait et al. 2002)
300 ppm Ag, 400 ppm Au. (Cu,Ag)2Se, AgCuSe, Ag2Se, Ag, Au, La Caridad refinery of Mexicana de Cobre (Chen and
Ag3AuSe2 Dutrizac 2005)
0.1–2% Au, 4–25% Ag. Canadian copper anode slimes
Ag2O~5.9%, Au~0.22% Au8Ag2Te2, Ag2Se, AgTe, Ag3Au Te2, Sarcheshmeh copper complex in Iran (Khaleghi et al.
AuAgTe4, AgCl 2014)
10.45% Ag, 0.21% Au, 0.03% Pt Ag2Se, Ag2Te, Au, Pt Daye Nonferrous Metal Co., Ltd. China. (Li et al. 2015)
2.62% Ag, 157 g/t Au, 27.6 g/t Pt, Ag2Se, AgCu4(AsO4)3 A copper-nickel refinery, China. (Lu et al. 2015)
95.5 g/t Pd.
2.60% Ag Ag2Se Gansu Province China. (Yang et al. 2015)
0.099% Au, 2.2% Ag Ag2SO4 China (Ding et al. 2017)
3.8% Rh, 10% Ru, 0.21% Ir, 0.06% Rh, Ru, Ir, Pt, Pd Concentrated residue (Nagai et al. 2017)
Pt, 0.02% Pd.
103.2 g/L Au, 4124.7 g/L Ag, Au, Ag, Pd China (Yang et al. 2017b)
87.0 g/L Pd
0.133% Au, 2.054% Ag Au, AgSbO3, Ag2SO4 Sarkuysan Co. Turkey (Donmez et al. 2001)
4.59% Ag, 1.5% Au Ag, Au Korea company (Xing and Lee 2017)
Tin anode slimes 12% Ag Ag, Ag3Sn Sungeel Hi-Tech. Ltd., Gunsan, Korea (Han et al. 2015)
3% Ag Ag, Ag4Sn Electrorefining of Sn-Ag-Cu (SAC alloy) (Harangi et al.
2015)
0.31% Ag Ag A Tin refinery China. (Lu 2015)
0.002% Au, 0.15% Ag Ag, Au China (Han et al. 2017)
Zinc anode slimes 0.176% Ag AgCl, Ag2O3, AgNO3(Ag6O8) Zhuzhou Smelter Group Co., Ltd. China (Xiang et al.
2012)
Lead anode slimes 1.08%Ag, 2.35 g/t Au Ag3Sb, Au Hechi smelter of Huaxi Group Corp. in Guangxi, China
(Cao et al. 2010)
Hunan province in China (Lin and Qiu 2011)
12.88 wt% Ag, 0.071 wt% Au, / (Arai et al. 1990)
0.0015 wt% Pt, 0.052 wt% Pd

percentage of noble metals in copper anode slimes, many
technologies have been proposed for the removal of base
metals and the enrichment of the noble metals.
In the pyrometallurgical treatment for the copper anode
slimes, base metals and mattes with low viscosity such as Ni,
Sn, and Zn can form alloys with noble metals at high tem-
perature around 900–1200°C and these alloys can be easily
separated from the slags (Chen and Huang 2007; Safarzadeh
et al. 2018). Some hydrometallurgical methods are also
employed to enrich noble metals in the residue by dissolving
most of the base metals by acidic or alkaline solution at lower
than 100°C. For these purposes, inorganic acids like sulfuric
acid (Zheng et al. 2010), 4 M nitric acid (Antipov and Tarasov
2002; Khaleghi et al. 2014), 4 M hydrochloric acid (Zheng and
Hong 2011; Wang et al. 2014), and some alkaline solution
with 4 M NaOH or alkaline fusion-leaching with NaOH/slime
mass ratio of 2 (Kilic et al. 2013; Li et al. 2015, 2016) are
employed for the removal of Cu, Se, Sn and so on. In some
cases, inorganic acids alone are not sufficient to dissolve the
metallic alloys between noble metals and base metals.
Therefore, several physical methods are employed to destroy
the structures of these compounds and to enhance the leach-
ing of noble metals. There are several leaching methods such
as high pressure and high temperature (Chen 2008), alkaline
pressure oxidative leaching for the removal of As and Se at
200°C (Liu et al. 2014), soda roasting-alkaline leaching such as
Na2CO3 or NaOH in the temperature range of 300–700°C and
acid leaching (Guo et al. 2015; Lu et al. 2015), and microwave
with 2.45 GHz multimode cavity (Yang et al. 2015).
Meanwhile, in order to improve the leaching efficiency of
metals, some oxidizing agents are added to the inorganic acid,
such as oxygen gas (Donmez et al. 1998; Havuz et al. 2010), MnO2
(Hait et al. 2002), NaClO, NaClO3, H2O2, and HNO3(Xing and
Lee 2017). The leaching reactions for each system are displayed in
Table 2. For some complicated copper anode slimes, the enrich-
ment of noble metals by removing base metals requires several
stages such as first leaching of Cu and Te by sulfuric acid and
second leaching of the noble metals by HCl in the presence of
H2O2, and then the following steps include respective leaching by
NaOH, H2SO4, and roasting for the removal of the remaining base

Table 2. The corresponding reaction of noble metals in the anode slime in different conditions.
Conditions Reactions References
H2SO4 + O2 2CuAgS(s) + 2H2SO4(aq) + O2(aq) → 2CuSO4(aq) + Ag2S(s) + S(s) + 2H2O (Donmez et al. 1998)
Cl2 Au(s) + 3/2 Cl2(g) + Cl−(aq) → AuCl4−(aq) (Donmez et al. 1999; Donmez et al. 2001)
MnO2 + NaCl + H2SO4 MnO2 + 2NaCl + H2SO4 → MnSO4 + Na2SO4 + Cl2 + H2O (Hait et al. 2002)
Ag2Se + Cl2 + H2O → AgCl ↓+H2SeO3 + HCl
HNO3 2Ag2Se + 8HNO3 = 2AgNO3 + Ag2SeO3 + H2SeO3 + 3NO2 + 3NO + 3H2O (Antipov and Tarasov 2002)
Na2CO3 + O2 Ag2Se + Na2CO3 + O2 = Na2SeO3 + 2Ag + CO2 ↑ (Lu et al. 2015)
Ag2Se + Na2CO3 + 1.5O2 = Na2SeO4 + 2Ag + CO2 ↑
Ag2Te + Na2CO3 + 1.5O2 = Na2TeO4 + 2Ag + CO2↑
 MINERAL PROCESSING AND EXTRACTIVE METALLURGY REVIEW 3

Copper anode slime base metals such as lead, antimony, and tin are removed by
Cu, Te vacuum carbothermal reduction at 950°C with chamber pres-
sure at 10–25 Pa (Li et al. 2013), acid and alkaline pressure
H2SO4 leaching Cementation Cu oxidative leaching with 2.5 M NaOH at 130°C and sulfidation
roasting at 1050°C (Lu 2015; Han et al. 2017), respectively.
These methods have some advantages in terms of lower
HCl/H2O2 Te, Se, Rh,Ru NaOH leaching Te energy consumption, less pollution, and higher recovery
efficiency.

Residue (Rh, Ru,

Au extraction 2.4. Zinc anode slimes
Te, Se, Cu)
There are only a small amount of Ag in the zinc anode slime
and few works have been reported on the recovery of noble
SO2 solution NaOH/Air leaching Se,Te
metals from these anode slimes. The main components are
MnO2, PbSO4, and PbO2 and silver exists as AgCl, Ag2O3, and
Ag7NO3(Ag6O8). Xiang et al. (Xiang et al. 2010) employed the
Pt, Pd H2SO4 leaching Cu system of flotation-high gradient magnetic separation-shaking
table to obtain high grade silver concentrate and anglesite
concentrate. The recovery of silver and lead from the zinc
Cl2/C volatilization Se, Te anode slimes was above 74% and 84%, respectively. It was
shown that the presence of SO42− and the solution pH have an
important effect on the reaction behavior of silver during the
NaCl, C/Cl2 flotation (Xiang et al. 2012).
Roasting

2.5. Flotation of noble metals

H2O dissolution
Rh and Ru solution
Figure 1. Process for concentration and recovery of precious metals.
metals. The details are shown in Figure 1 (Nagai et al. 2017).
Consequently, the different noble metals are collected in the
several residues for further recovery.
2.2. Lead anode slimes
Lead anode slimes contain base metals such as Pb, Sb, As, Cu,
and Bi (Cao et al. 2010) and a small amount of silver and gold
which exist as various compounds as shown in Table 1. It is
difficult to directly dissolve noble metals from these anode
slimes. Among the base metals, arsenic is very harmful to the
environment and thus some pretreatments like vacuum
dynamic evaporation, vacuum dynamic flash reduction (Lin
and Qiu 2012), and alkaline oxidative leaching (Liu et al.
2013) are firstly employed to remove As with 2 M NaOH
and H2O2/slimes ratio of 0.2 at 80°C. When the amount of Sb
is considerable, chlorine gas with two stages is employed for
the separation of Sb and As with solution potential of 450 mV
at 120°C (Cao et al. 2010). Therefore, some corrosion-resis-
tant materials should be used for the reaction vessel, which
needs high investment.
2.3. Tin anode slimes
In tin anode slimes, silver, gold, and other noble metals exist
as metallic silver, gold, and AgxSn. To enrich noble metals, the
C
Flotation is an effective method for concentrating of metals
from various minerals containing low grade noble metals.
Noble metals are generally covered by some impurities such
as Te, Se, and Tb (see Table 1). These compounds are readily
flotatable with some kinds of collectors like xanthate and
dithiophosphate. During the flotation, some modifiers, oxygen,
solution pH affect the flotation of the metals (Bulatovic 2010).
Some literatures reported that noble metals can be concen-
trated from anode slimes by flotation with xanthate and dithio-
phosphate or their mixture (Hukki and Runolinna 1950;
Ogunniyi and Vermaak 2009; Acarkan et al. 2010; Xiang et al.
2012; Chen et al. 2013). Above 99% of gold and silver could be
enriched into the concentrate with small parts of impurities by
using the xanthate collector of Reagent 208 (American Cyanamid
Company) along with the frother of DuPont B-23 from anode
slimes (Hukki and Runolinna 1950). The advantage of flotation is
to simplify and improve its efficiency in treating various anode
slimes. However, the disadvantages are the 5–10% carry-over of
Ni into the concentrate and the presence of excessive organic
chemicals like glue and oil might affect the flotation of metals.
Meanwhile, some home-made collectors were obtained by mixing
the potassium amyl xanthate and aminothiophenol in the pre-
sence of methyl isobutyl carbinol as a frother and Na2SiO3 as a
depressant, which were employed for copper anode slimes or
minerals (Acarkan et al. 2010; Chen et al. 2013). The results
indicate that the flotation increased the concentration of gold
and silver to 5–100 times compared to the raw anode slimes.
3. Leaching of noble metals after pretreatment of
the anode slimes
Leaching of the enriched residues containing noble metals is an
important step for the recovery of noble metals. The enriched
4 W. D. XING ET AL.
residues of lead, tin, and zinc anode slimes generally contain
only either gold or silver among the noble metals. Therefore,
leaching of these enriched residues with nitric acid solution
would lead to the recovery of silver metal, while dissolving
most of the base metals (Li et al. 2006; Harangi et al. 2015).
In contrast, other noble metals are present in the enriched
residues of copper anode slimes, which makes the separation
process complicated. Therefore, leaching of noble metals from
the enriched residues of copper anode slimes after pretreat-
ments is considered in the following sections. Leaching
reagents such as cyanide, thiourea, thiosulfate, and halide
have been employed for this purpose and thus the character-
istics of these systems are reviewed.
3.1. Cyanide leaching
Since the leaching kinetics of gold by cyanide is slow at room
temperature, high temperature, and/or pressure and catalysts
are needed to improve the reaction kinetics (Senanayake 2004;
Chen and Huang 2006; Oraby and Eksteen 2015). The leach-
ing behavior of noble metals could be represented as
Equations (1) to (4). However, the metal complexes with
CN− might be decomposed when reaction temperature is
above 180°C, which is represented in Equations (5) and (6)
(Chen and Huang 2006). Therefore, the control of reaction
temperature is important in cyanide leaching.
4Au þ 8CN þ O2 þ 2H2 O ! 4AuðCNÞ
2 þ 4OH

(1)
2Me þ 8CN þO2 þ2H2 O ! 2MeðCNÞ2
4 þ4OH
 metals and thus hinders the leaching of noble metals.
(2)
ðMe ¼ Pt; Pd:Þ
4Rh þ 24CN þ3O2 þ6H2 O ! 4RhðCNÞ3
4 þ12OH

(3)
Au þ CuðCNÞ2  þ4NHþ
4 þ0:5O2 þ2OH
 Thiourea as an alternative reagent for cyanide can form
! AuðCNÞ 2þ
2 þCuðNH3 Þ4 þ2H2 O (4)
MeðCNÞ2
4 þ1:5O2 þ7H2 O
! Me þ 4NH3 þ4CO2 þ2OH ðMe ¼ Pt; PdÞ (5)
2RhðCNÞ3
4 þ4:5O2 þ21H2 O
! 2Rh þ 12NH3 þ12CO2 þ6OH (6)
The presence of specific metals ions has been shown to affect
the dissolution of metals. While small amounts of Hg (10−5 M),
Ag and Pb ions could reinforce the leaching of gold in the
cyanide solution (Jeffrey and Ritchie 2000; Zhong et al. 2018),
copper could increase the consumption of cyanide and thus
decrease the dissolution rate of gold (Jiang et al. 2001). In the
system of thiocyanate-cyanide for the leaching Pt and Pd, iron
(III) as an oxidant accelerates the dissolution of Pt and Pd and
enhance the formation of the complex of Pt(IV) and Pd(II)
with cyanide and thiocyanate ions (Shaik and Petersen 2017).
In addition, glycine can improve the dissolution of gold when
the concentration of cyanide is very low (Oraby and Eksteen
2015). The mechanism was explained in Equation (8), which
can decrease the consumption of cyanide. However, the severe
environmental burden and the toxicity related to cyanide limit
the application of this leaching process industrially.
Auþ þ2ðH3 NCH2 COOÞ $ AuðNH2 CH2 COOÞ
2 (7)
4Au þ 8NH2 CH2 COOH þ 4OH þO2
(8)
! 4AuðNH2 CH2 COOÞ
H2 O2
2 þ6H2 O
3.2. Thiosulfate leaching
Compared with cyanidation in the gold leaching, thiosulfate
has many advantages in terms of reaction selectivity and low
corrosivity to equipment. The presence of NH3, Cu2+, and
Ag+ has a favorable effect on the dissolution of gold by
thiosulfate solution (Aylmore et al. 2014), while Zn, Cd, Co,
Cr, and Ni suppress the dissolution of gold and increase the
consumption of thiosulfate (Feng and Deventer 2002;
Aylmore 2016). Furthermore, during the leaching of decop-
perized anode slime, it was found that Pb has some deleter-
ious effects on the dissolution of gold and silver and increase
the consumption of thiosulfate (Xu et al. 2016). This might be
attributed to the fact that PbO covers the surface of noble
Therefore, measures should be taken to reduce the concentra-
tion of Pb(II) below certain level before the recovery of noble
metals.
3.3. Thiourea leaching
strong complexes with gold(I). Therefore, leaching of gold
by thiourea has been investigated in the presence of an
oxidizing agent (Ubaldini et al. 1998; Li and Miller 2006;
Chang et al. 2017). Yavuz et al. (Yavuz and Ziyadanogullari
2000) investigated the leaching of gold by thiourea solution
from a complex anode slime. It was found that thiourea is
easily decomposed in the presence of other base metals,
resulting in an increase in the consumption of leaching
agent. Moreover, sulfur can precipitate Ag2S, which passi-
vates the surface of gold (Yavuz and Ziyadanogullari 2000;
Amer 2002, 2003). This situation is encountered in the
leaching of silver by thiourea in the presence of ferric ion
as an oxidizing agent. The detailed complex reaction of
metals with thiourea are shown in Equations (9) and (10)
and Equations (11)–(14) refer to the decomposition reac-
tions of thiourea (Tremblay et al. 1996; Kai et al. 1997; Amer
2003; Kasim et al. 2011; Ranjbar et al. 2014; Chang et al.
2017; Xing et al. 2017). Owing to these disadvantages of
thiourea, few systems have been employed for the treatment
of anode slimes.
 MINERAL PROCESSING AND EXTRACTIVE METALLURGY REVIEW 5

Au þ 2CSðNH2 Þ2 þFe3þ , Au½CSðNH2 Þ2 þ

2 þFe
2þ
(9) the concentration of sodium in the waste solution high, which
has serious effect on the environment.

2Au þ ClO þ
3 þ6H þ7Cl

! 2AuCl
4 þ3H2 O (20)
Ag þ 3CSðNH2 Þ2 þFe 3þ
, Ag½CSðNH2 Þ2 þ
3 þFe
2þ
(10)
Ozone was employed as an oxidizing agent in HCl solution to
dissolve Au and Pd, the reactions of which are represented as
Equations (21) and (22) (Viñals et al. 2006). In the presence of
2SCðNH2 Þ2 þ2Fe3þ , ½SCðN2 H3 Þ2 þ2Fe2þ þ2Hþ (11)
H2O2, Pd and Au are dissolved in a similar fashion into the
HCl solution as represented in Equations (23)–(26). In addi-
tion, chloride ions can be oxidized to chlorine gas by H2O2
2SCðNH2 Þ2 þH2 O2 ! ½SCðN2 H3 Þ2 þ2H2 O (12) (Harjanto et al. 2006). Other works have reported on the use
of NaClO, HClO4, and HClO as an oxidizing agent or the
substitution of Cl ions and it was found that H2O2 is the most
ðSCN2 H3 Þ2 ) CSðNH2 Þ2 þNH2 CN þ S (13) effective as an oxidizing agent in the dissolution of PGMs and
cannot be completely replaced by NaClO (Cao et al. 2006;
Harjanto et al. 2006; Xing and Lee 2017).
2Agþ þ ðNH2 Þ2 CS þ 2OH ¼ Ag2 S þ NH2 CN þ 2H2 O (14)
Au þ 1:5O3 þ3Hþ þ4Cl ! AuCl
4 þ1:5O2 þ1:5H2 O (21)

3.4. Halide leaching PdþO3 þ2Hþ þ4Cl ! PdCl2

4 þO2 þH2 O (22)
In order to dissolve gold by halogen acid, the presence of an
oxidizing agent such as NaClO, NaClO3, H2O2, and HNO3 is
necessary. HCl first reacts with these oxidizing agent to form a PdþH2 O2 þ4HCl $ H2 PdCl4 þ2H2 O (23)
stronger oxidizing agents which can easily dissolve gold
(Marsden and House 2009; Xing and Lee 2017). Moreover,
chlorine gas was also employed for the recovery of noble
H2 O2 þ2HCl $ Cl2 þ2H2 O (24)
metals from the copper anode slime (Donmez et al. 1999,
2001). Chlorine gas first dissolves into water and the dissolved
chlorine gas oxidizes the gold which dissolves into the solu-
tion. The leaching reactions of gold and silver with chlorine Pd þ Cl2ðaqÞ þ2HCl $ H2 PdCl4 (25)
gas are represented as Equations (15)–(19) (Cooper 1990;
Donmez et al. 1999). Owing to the toxicity of chlorine gas,
the leaching vessel should be tightly closed against the leakage Pd þ HClO þ 3HCl $ H2 PdCl4 þH2 O (26)
of chlorine gas.
In the use of aqua regia for the dissolution of PGMs, nitric

Cl2ðgÞ þH2 OðlÞ Ð Hþ
ðaqÞ þClðaqÞ þHOCl (15) acid first reacts with HCl to form chlorine gas. Equations
(27)–(29) represent the reactions occurring in the aqua regia
system (Sheng and Etsell 2007; Hammadi et al. 2017). Since
HOCl Ð Hþ þClO (16) noble metals have a strong tendency to form complexes with
chloride ion, chlorine gas was electrolytically produced for the
dissolution of PGMs (Upadhyay et al. 2013). However, strong
AuðsÞ þCl  toxic gas NO or NO2 are produced in the dissolution of
ðaqÞ þ0:5Cl2ðgÞ ! AuCl2ðaqÞ (17)
metals, which has important effect on the work conditions
and the equipment. Similarly, some other halide reagents such
as bromide and iodide were investigated for the leaching of
AuCl 
2ðaqÞ þCl2ðgÞ ! AuCl4ðaqÞ (18) gold from the diverse resources (Konyratbekova et al. 2014).
However, some drawbacks like high cost of reagents, the high
requirements of corrosion-resistant equipment prevented the
Ag2 Se þ 3Cl2 ! 2AgCl # þSeCl4 (19) utilization of these systems.
The mixture of sulfuric acid and strong oxidants like NaClO3 HNO3 þ3HCl , NOCl þ Cl2 þ2H2 O (27)
was studied by Ding et al. (Ding et al. 2017) for the dissolution
of gold from decopperized anode slime of electronic waste and
the leaching reaction of gold is represented in Equation (20).
NOCl þ 2H2 O , HNO2 þHCl (28)
The gold was recovered by reduction with Na2SO3 in the
optimal pH of 1.75 by keeping the concentration of other
impurities low. However, hydrometallurgical methods results
in more residues and the employment of sodium salts makes 2Au þ 3HNO3 þ9HCl ! 2AuCl3 þ3NOCl þ 2H2 O (29)
6 W. D. XING ET AL.
4. Separation of noble metals from the leaching
solution
Some separation methods are applied to the leaching solution of
the enriched anode slime to recover the pure noble metals. These
methods include cementation (Donmez et al. 2001; Aktas 2011;
Coetzee et al. 2018), activated carbon adsorption (Chand et al.
2009; Snyders et al. 2015), solvent extraction, ion exchange,
electrowinning and adsorption by new materials such as silicon
organic polymer, metal-organic frameworks (MOFs) and photo-
reduction by UV light with various wavelengths.
4.1. Separation by cementation
Cementation is one of the most effective and economic tech-
niques for separation methods. The noble metal ions are
reduced by less noble metal such as zinc, iron, copper, and
aluminum (Aktas 2012; Kuntyi et al. 2013; Lee et al. 2013).
Gold was recovered by the reduction of copper disc from the
chloride leach liquor of anode slimes containing Au and Ag
along with some base metals like Pb, Sb, Zn, Cu, and Sn
(Donmez et al. 2001). A mechanistic study on the cementa-
tion of Ru(III), Rh(III), and Ir(IV) from sulfate solution by
using iron ion indicated that solution pH has the most sig-
nificant effect regardless of iron valence state (Coetzee et al.
2018). In recent work by Aktas (Aktas 2011), 99% of rhodium
(III) was recovered by zinc powder from the waste rinsing
water. However, the free acid and some other metal impurities
increase the consumption of zinc powder.
4.2. Separation by activated carbon
Activated carbon adsorption is a traditional method to
remove metal ions and commonly employed for the adsorp-
tion of gold from the cyanide solution. Snyders et al. (Snyders
et al. 2013, 2014, 2015) reported the recovery of Pt(II), Pd(II),
and Au(I) from cyanide solution by activated carbon. The
concentration of NaOH and NaCN and temperature have an
important effect on the elution of the three metals. In addi-
tion, pretreatment by HCl could improve the elution of Pt and
Pd, while the addition of KSCN has a deleterious effect. The
loading order of noble metal ions over the activated carbon
was Au(CN)2− > Pt(CN)42− > Pd(CN)42−. Chand et al. (2009)
found the porous carbon prepared by rice husk and barley
straw could selectively load precious metal ions from HCl
solution in addition to Cu(II), Ni(II), Fe(III), Pd(II), and Au
(III). Especially the rice husk carbon could efficiently separate
Au(III) from other metals. The HCl concentration has a little
Table 3. Stability constants of several complexes of gold(Fleming 1992; Schweitzer and Pesterfield 2010).
Gold(I) β2 Gold(III)
Au(CN)2̶ 2 × 1038 Au(CN)2̶
Au(S2O3)23̶ 5 × 1028 AuI2̶
Au(CS(NH2)2)2+ 2 × 1023 Au(SCN)4̶
AuI2− 4 × 1019 AuBr4̶
Au(SCN)2− 1.3 × 1017 AuCl4̶
AuBr2− 1012
AuCl2− 109
effect on the adsorption of noble metals by rice husk carbon
and barley straw carbon. Especially, the metals adsorbed on
the carbon could be recovered by burning the loaded carbon
materials.
In recent years, graphene oxide was applied to the adsorp-
tion of gold from the Au(CN)2̵̶ solution (Yang et al. 2017a).
Graphene with single or several atomic layered graphites has
excellent electrical, thermal, and mechanical properties. It was
found that the loading capacity of the graphene oxide was
three times as large as that of the activated carbon. The
adsorption and desorption performance of graphene oxide is
better than that of the activated carbon. However, compared
with activated carbon, graphene is more expensive and needs
the high-quality equipment and is difficult to control.
4.3. Separation by solvent extraction
Solvent extraction is widely employed to separate gold, silver,
and PGMs present in the leach liquor of anode slime, and
researchers have focused on the development of more efficient
extractants for the separation of metals with similar properties
(Kolarik 2000). In the case of gold and silver, much investiga-
tion has been published from different media, such as cyanide
(Chen et al. 2017), chloride (Kedari et al. 2006; Pan and
Zhang 2009; Yin et al. 2013; Ortet and Paiva 2015), nitrate
(Raj et al. 2006; Ahmed et al. 2011) thiosulfate (Zhao et al.
1999; Kejun et al. 2004), and thiourea(Kim et al. 1995; Arroyo
et al. 2008). In these works, acidic, neutral, and basic extrac-
tants as well as their mixtures are employed according to the
speciation of the metal ions (see Table 3). In the case of
PGMs, most of work has focused on the extraction behavior
from chloride solution (see Table 4). The extraction order by
basic extractants is MCl4− > MCl62− > MCl42− > MCl63− >
aquo species (Warshawsky 1983; Yu 2004; Bernardis et al.
2005).
Separation of gold from leach liquor of copper anode slime
was investigated by Sadeghi et al. (Sadeghi and Alamdari
2016) using TBP. The coextracted impurities like Fe, Cu, Se,
and Pd can be scrubbed by distilled water before gold strip-
ping using sodium thiosulfate, and then gold particles can be
obtained by reduction with SO2. TBP was also tested to
separate Ir(IV) and Rh(III) from a chloride solution in the
presence of stannous chloride (Zou et al. 2004). In this system,
SnCl2 first reduce IrCl62− into IrCl63− which cannot be
extracted by TBP. At the same time, RhCl63− is reduced to
Rh(I), which can be extracted by TBP. The detailed solvent
extraction reactions are represented as Equations (30)
and (31).
β4 Silver(I) βn Silver(I) βn
1056 Ag(CN)2− 1020.9 AgCl2− 103.3
5 × 1047 Ag(CN)32− 1021.8 AgCl32− 102.3
2 × 1042 Ag(SCN)− 2 × 108 AgBr2− 107.7
2 × 1032 Ag(SCN)32− 3.2 × 109 AgBr32− 108.7
2 × 1026 Ag(SCN)43− 5.66 × 109 AgI2− 1011.7
Ag(S2O3)− 108.82 AgI32− 1013.1
Ag(S2O3)23− 1013.83

Table 4. PGMs species in chloride solution (Bernardis et al. 2005).
Palladium Species
Pd(II) [PdCl4]2−
Pd(IV) [PdCl6]2−
Ruthenium Species
Ru(III) [RuCl6]3−, [RuCl5(H2O)]2−
[RuCl4(H2O)2]−,[RuCl3(H2O)3]
Ru(IV) [RuCl6]2−,[Rh2OCl10]4−
[Ru2OCl8(H2O)2]2−
Iridium Species
Ir(III) [IrCl6]3−, [IrCl5(H2O)]2−
[IrCl4(H2O)2]−
Ir(IV) [IrCl6]2−
4TBPo þ 4Hþ
aq ! 4ðHTBPÞo
½Rh2 Cl6n ðSnCl3 Þn 4
aq þ 4HTBPo
 
! ðHTBPÞ4 ½Rh2 Cl6n ðSnCl3 Þn 4
0 n ¼ 2e 4
Acidic extractants, Cyanex 272 and LIX 63 were employed to
separate Au(III), Pd(II), and Pt(IV) from the leaching solution
of copper anode slime by HCl and H2O2 (Xing et al. 2018a).
Au(III) was selectively extracted over Pd(II) and Pt(IV) by
Cyanex272, while LIX63 could selectively extract Pt(IV) over
Au(III) and Pt(II). Therefore, the three noble metals can be
efficiently separated from each other by solvent extraction
with Cyanex 272 and LIX 63. Moreover, most of Au(III)
was extracted over other base metals from the synthetic
leach liquor of anode slime by Cyanex272 (Xing et al.
2018b). (NH4)2S2O3 and NH2SCN can strip the Au(III)
from the loaded Cyanex 272. A mixture of N1923 (methyloc-
tadecyl amine) with either TBP or TRAO was employed to
separate gold from the thiosulfate leaching solution of anode
slime, indicating that TRAO was more effective in separating
gold than TBP (Zhao et al. 1999).
The solvent extraction performance can be improved by
firstly adding some agents such as sugar into aqueous solution
in the separation of Pt(IV), Pd(II), and Rh(III)(Zhang et al.
2012a). It was found that the added sugars can form three-
liquid-phase extraction.
4.4. Separation by electrowinning
Electrowinning has been employed for the purification and
recovery of metals from the cyanide solution (Barbosa et al.
2001; Paramguru 2002; Steyn and Sandenbergh 2004; Yap and
Mohamed 2007). The separation of gold by electrowinning
was achieved from the thiourea-H2SO4 solutions (Juarez and
Dutra 2000). The results showed that most of Au-thiourea
species was firstly adsorbed on the electrode surface and then
reduced into metal. The increase in thiourea concentration
can decrease the grain size of the deposited gold. Although
high temperature has a favorable effect on the gold recovery,
the stability of thiourea at this condition should be consid-
ered. Urbanski et al. also verified the feasibility of the electro-
winning of gold from thiourea solutions in the presence of
alcohol (Urbanski et al. 2000). In this system, the role of
alcohol was to protect the oxidation of thiourea at the
MINERAL PROCESSING AND EXTRACTIVE METALLURGY REVIEW 7
Rhodium Species
Rh(III) [RhCl6]3−, [RhCl5(H2O)]2−
[RhCl4(H2O)2]−
Rh(IV) [RhCl6]2−
Platinum Species
Pt(II) [PtCl4]2−
Pt(IV) [PtCl6]2−
Osmium Species
Os(IV) [OsCl6]2−
(30) anode. The possible electrowinning reaction may be repre-
sented as
Au½CSðNH2 Þ2 þ
2 þe

! Au þ 2CSðNH2 Þ2 (32)
Chatterjee (Chatterjee 1996) studied the recovery of gold by
(31) electrowinning from as-cast bars of wohlwill anode slime in
hydrochloric acid electrolyte. Among the process, the oxida-
tion state of gold was kept at trivalent by blowing air slowly.
Moreover, the gold sorption mechanism in the electrochemi-
cal process was studied in the HCl solution (Alorro et al.
2015). The detailed results indicated that AuCl4− was
adsorpted on the magnetite surface by electrostatic attraction
and reduced into metallic Au. Meanwhile, the Fe3+ produced
from magnetite could affect the adsorption of gold. Arai et al.
(Arai et al. 1990) reported the recovery of silver by electro-
winning process from the nitric acid leaching solution on lead
anode slimes. Silver can be completely separated by employ-
ing HCl solution and metallic silver was obtained from the
thiocyanate solution of AgCl thus obtained by electrowining.
The presence of Ag(SCN)nn−1 in thiocyanate solution could
increase the production of metallic silver with purity higher
than 99.5%. The disadvantages of this process are the com-
plexity, high consumption of chemicals, as well as the neces-
sity of another process for the recovery of Au, Pt, and Pd.
4.5. Separation by ion exchange
Ion exchange is widely employed to recover and purify gold,
silver, and PGMs from diverse aqueous solutions (Shams
2004; Silva et al. 2018). Table 5 lists the nature of resins
employed for the purification of precious metal ions from
different medium. In the case of chloro-complexes in Tables
3 and 4, the predominant species of noble metals are anion
and thus anion exchange resins are generally selected. The
adsorption order among the chloro-complexes is in the fol-
lowing order: MCl4− > MCl62− > MCl42− > MCl63− > aquo
species (Nikoloski and Ang 2013). However, the adsorption
mechanism of metal ions during ion exchange depends on the
nature of the noble metals. In the separation of Pt(IV) and Pd
(II) from cyanide leach liquor by ion exchange, it was found
that strong-base anion exchange resins with larger function-
alities and lower loading capacity can load more noble metal
ions and the presence of Zn(II) and Ni(II) affects more the
adsorption of Pd(II) into these resins than that of Pt(IV)
(Schoeman et al. 2017).
 8
W. D. XING ET AL.

Table 5. Adsorption of noble metals from different medium by ion exchange.

Resin Type Functional group Ions Media Eluant Refs.
717 resin Anionic Quaternary ammonium Ag(I),Au(III), Pd(II), Pt(IV) HCl (pH = 3) Thiourea + HCl (Liu et al. 2009)
Amberlite XAD7HP Nonionic Nonionic Au(III) Cu(II) pH = 0 HCl in acetone (Kim et al. 2011)
Bonlite BA304 Anionic R-CH2N+(CH3)3/type1quaternary ammonium Au(III) Cu(II) pH = 0–14 HCl in acetone (Nguyen et al. 2010)
Purolite A-500
Duolite GT-73 Au(III),Pd(II) HCl / /
Lewatit MP-64 Anionic Tertiary/quarternary amine Au(III) HCl Acide thiourea (Alguacil et al. 2005)
Lewatit MonoPlus MP600 Anionic Type 2 quaternary ammonium/polyamine Pt(IV), Pd(II), Ir(III) HCl Acidic thiourea for Pt and Pd (Nikoloski et al. 2015)
Purolite S985
DEAE-cellulose Anionic Ionizable tertiary amine Au(III) HCl / (Tasdelen et al. 2009)
LMCCR Anionic Amino Pt(IV), Pd(II), Au(III) HCl Thiourea + HCl (Fujiwara et al. 2007)
PS-APD / Alcohol hydroxyl group Au(III) HCl / (Sun et al. 2011)
GMCCR / R-NH2 Au(III), Pt(IV), Pd(II) HCl Thiourea + HCl (Ramesh et al. 2008)
Purolite A-100 Anionic Tertiary amine Au(I) Cyanide Potassium hydroxide and potassium cyanide (Gomes et al. 2001)
NOTREN Anionic Quaternary ammonium Au(I), Ag(I) Cyanide / (Dicinoski et al. 2000)
TEA-BE
XZ-91419 Anionic M-+NR3X‾ Au(I) Cyanide Acidic thiourea (Hedjazi and Monhemius 2014)
Amberlite PWA-5 Au(I), Pt(II), Pd(II) Cyanide Potassium thiocyanate (Schoeman et al. 2012)
Bayer AP-247 Anonic Type1quaternary ammonium Au(I) Cyanide Thiocyanate (Oliveira et al. 2008)
Purolite A500 Nitrate solutions
Dowex 21K XLT Anionic Trimethyl/dimethyl ethanol/triethyl ammonium Pt(II), Pt(II) Cyanide (Schoeman et al. 2017)
Amberjet 4600
Amberlite PWA5
Minix
Purolite A500 Anonic Type1quaternary ammonium Au(I) Thiosulfate Chloride +sulfite (Jeffrey et al. 2010)
AuRIX100 Anionic Guanidine groups Au(I) Thiosulfate (Chaparro et al. 2015)
AV-17-10P Anionic Quaternary amino Ag(I) Thiosulfate, Thiocyanate Sulfuric acid/thiourea (Kononova et al. 2007)
VBC/DVB Anionic Quaternary ammonium Au(I), Ag(I) over Cu(II) Ammonium buffer / (Rabiega and Trochimczuk 2014)
NOTREN = synthesized by capping a tris(2-aminoethy)amine(TREN)resin derivative; TEA-BE: synthesized by forming a tribenzyl ether of tris(2-hydroxyethyl)amine(TEA) resin derivative; LMCCR: L-lysine modified crosslinked
chitosan; PS-APD: polystyrene-supported 3-amino-1,2-propanediol; GMCCR: glycine modified crosslinked chitosan resin; VBC/DVB: vinylbenzyl chloride/divinylbenzene.

In addition, the complexes of PGMs in the solution are
very complicated due to the hydrolysis and aquation reaction
which depends on the medium acidity and concentration of
chloride ions as shown in Table 4 (Colombo et al. 2008;
Kononova et al. 2010). Furthermore, the diversity of metal
oxidation state and formation of polynuclear compounds
complicate the adsorption behavior. In the chloride and sul-
fate-chloride solution, a series of works have investigated the
adsorption of Pt(II, IV) and Rh(III) by several anion exchange
resins like Purolite A500, AM-2B, Purolite S985 and etc.
(Kononova et al. 2010, 2011, 2012). The results demonstrated
that the adsorption kinetics of metal complexes are limited by
the gel diffusion and ion exchange equilibrium. Moreover,
platinum complexes have more affinity to the anion resins
than rhodium complexes in the system of sulfate-chloride
solution and the aged solution has some influence on the
adsorption of metal complexes due to the formation of some
metal species with H2O. The elution of gold thiosulfate from
resins was enhanced by employing sulfite in a base eluant
(Jeffrey et al. 2010). The sulfite reduced the affinity of gold for
the strong anion exchange resins, which leads to the elution of
gold. Moreover, the resins can be effectively reutilized after
elution for next adsorption stage.
4.6. Separation by other techniques
In recent years, several novel nanostructured materials such as
colloidal particles, porous micron sized grains, and mem-
branes have been developed. These materials have large sur-
face-to volume ratio and can be easily separated from a
dispersed medium by either sedimentation or an external
magnetic force, which makes these material suitable for
usage in separation (Claesson and Philipse 2007). Some
works have reported on the separation of precious metals
from aqueous solution by nano-Al2O3 (Zhang et al. 2012b;
Wang et al. 2015), amine-modified tannin gel (Morisada et al.
2011), mesoporous silica (Zheng et al. 2012; Fotoohi and
Mercier 2015), and membrane (Estay et al. 2013). In the
case of recovery of precious metals, a silicon organic polymer
containing PSOT-3(dioxothiocarbamide groups) was investi-
gated for the adsorption of gold in HCl solution (Yunden et
al. 2017). It was found that the optimum loading condition is
only limited in the range of 0.1–0.3 M HCl. The advantage is
that the adsorption capacity is in direct proportion to the
initial gold concentration. The PSOT-3 is synthesize as
shown in Equation (33) and the adsorption process of Au
(III) can be described as Equation (34).
2nH2 O2
N½ðC2 H5 OÞ3 SiðCH2 Þ3 NH2 CS
6nC2 H5 OH
! ½O1:5 SiðCH2 Þ3 ðNHÞ2 CSO2 n (33)
R  CH2 SiO1:5 (34)
MINERAL PROCESSING AND EXTRACTIVE METALLURGY REVIEW 9
Photoreduction as a clean technique was tried for the
separation of Pd(II) and Ru(III) in high level liquid wastes in
the presence of alcohols (Li et al. 2017). The results indicated
that chloride ion and low pH have a negative influence on the
reduction of Pd(II) and Ru(II). Moreover, Pd(II) and Ru(II)
could be separated over Nd(III) by controlling the wavelength
of UV light. However, this method requires a strict control over
the solution conditions and equipments. Meanwhile, the feasi-
bility is not clear in the presence of other base metals.
MOFs are a type of porous coordinated polymer with one-,
two-, or three-dimensional structures, which can be designed to
obtain some special structures with excellent properties such as
storage and separation (Rosi et al. 2003). The MOFs like Zr-
cluster-based was employed for the separation of Au(III), Pt
(IV), and Pd(II) from the acid solution of pH 1 (Lin et al.
2017). At present, most of MOFs is not stable in water and thus
further work should be done to overcome this drawback for
their application to the separation of metals.
5. Conclusions
Recovery of noble metals from various anode slimes is impor-
tant not only from the viewpoint of environmental protection
but also for secondary resource utilization. Anode slimes
result from the electrorefining of copper, lead, tin, and zinc.
Gold and sliver are distributed in each anode slime but PGMs
are mostly found in copper anode slimes.
Pretreatment of anode slimes is necessary to remove the
base metals in the outlayer of the anode slimes and thus
concentrate the noble metals. Pyrometallurgy and hydrome-
tallurgy are generally combined to treat anode slimes contain-
ing alkaline, acid leaching, and roasting with additional
assistants from oxidizing agent, high pressure, vacuum, ultra-
sound, and microwave. The concentrates containing noble
metals are dissolved by diverse aqueous solutions such as
cyanide, thiosulfate, thiourea, and halide. Among these solu-
tions, thiosulfate is considered as an alternative for cyanide in
the dissolution of gold. Hydrochloric acid is adequate for the
dissolution of PGMs in the presence of H2O2.
Separation of noble metals from the leaching solution is a vital
step for the recovery of noble metals with high purity.
Cementation, activated carbon adsorption, and solvent extraction
have been employed in the industries for many years.
Electrowinning and ion exchange are mainly used for the purifi-
cation of metals from the solutions. In recent years, new materials
such as graphene, nanoparticles, and MOFs are employed for the
separation of noble metals. However, more work should be done
to elucidate the reaction mechanism and its applicability for the
recovery of noble metals from anode slimes.
Disclosure statement
The authors report no conflicts of interest. The authors alone are
responsible for the content and writing of the article.
Funding
This work was supported by National Research Foundation of Korea
(2018R1D1A1B07044951).
10 W. D. XING ET AL.
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