INDONESIAN MINING JOURNAL Vol. 20, No.

1, April 2017 : 31 - 38

EXTRACTING SILVER FROM ANODE SLIME

AFTER LEAD AND GOLD SEPARATIONS
EKSTRAKSI PERAK DARI LUMPUR ANODA SETELAH
PEMISAHAN TIMBAL DAN EMAS

ISYATUN RODLIYAH and SITI ROCHANI

Research & Development Centre for Mineral and Coal Technology
Jalan Jenderal Sudirman 623 Bandung 40211
Ph. (+6222) 6030483, Fax. (+6222) 6003373
e-mail: isya@tekmira.esdm.go.id

ABSTRACT

Anode slime, a byproduct from the process of copper electrorefining into the copper cathode, contains
several valuable elements that can be extracted after Cu and Pb separations. Another alternative route
for extracting the precious metals is still needed in terms of gaining more economical route. This research
aims to seek the new route to extract the precious metals, especially silver from anode slime. In these
experiments, the anode slime was obtained from PT Smelting Gresik. The lead was separated to produce
the residue which was then chlorinated to extract the gold. Later the residue was used for extracting the
silver by dissolving it in ammonium hydroxide solution with varying time dissolutions and concentrations
and later dissolving in hydrochloric acid to form silver chloride which was reduced to metallic silver. These
experiments had two trials. The first one related to directly using residual chlorination after gold separation
and the second one employed the same residual chlorination but processed through de-chlorination by
adding sodium carbonate. The result showed that the highest silver recovery of 53.56% related to 5 M
ammonium hydroxide concentration, the temperature of 30°C, dissolution time of 60 minutes. Recovery of
53.78% was achieved at 7 M ammonium hydroxide, the temperature of 30°C, dissolution time of 60
minutes. The feed of those experiments came from direct residual chlorination, while chlorination residue
that underwent de-chlorination produced silver recovery of 94.95% with leaching conditions of 5 M
ammonium hydroxide, the heating temperature of 30°C and leaching time of 60 minutes. The latest
recovery was relatively high resulted in the process could be scaled up to a continuous system.

Keywords: anode slime, silver recovery, silver extraction, chlorination process.

ABSTRAK

Sebagai hasil samping proses elektrorefining tembaga menjadi tembaga katoda, lumpur anoda yang
mengandung unsur berharga ini dapat diekstrak setelah memisahkan tembaga dan timbalnya terlebih
dahulu. Secara komersial, pemisahan logam berharga telah dilakukan, namun masih diperlukan rute
alternatif yang lebih ekonomis. Penelitian ini bertujuan untuk mendapatkan rute baru dalam mengekstrak
logam berharga terutama perak menggunakan lumpur anoda dari PT Smelting Gresik. Setelah
dipisahkan timbalnya kemudian diklorinasi untuk memisahkan emasnya. Residu hasil klorinasi digunakan
untuk ekstraksi perak dengan melarutkan residu dalam amonia dengan variabel konsentrasi dan waktu
pelarutan, kemudian menambahkan asam klorida sehingga terbentuk perak klorida yang selanjutnya
direduksi menjadi logam perak. Pada percobaan ini dilakukan dengan 2 cara yaitu residu klorinasi
pemisahan emas langsung diekstraksi dengan NH4OH dan residu klorinasi yang sebelumnya diproses
melalui deklorinasi dengan menambahkan natrium karbonat. Hasil percobaan menunjukkan perolehan
perak tertinggi sebesar 53,56% pada NH4OH 5M, suhu 30°C, waktu pelarutan 60 menit dan perolehan
sebesar 53,78% pada NH4OH 7M, suhu 30°C, waktu pelarutan 60 menit untuk residu langsung dari sisa
klorinasi. Residu klorinasi yang diproses melalui deklorinasi terlebih dahulu sebelum dilarutkan dengan
amoniak menghasilkan perolehan perak sebesar 94,95%. Kondisi pelarutannya adalah NH4OH 5M, suhu
30°C, waktu pelarutan 60 menit. Perolehan yang relatif tinggi ini dapat ditingkatkan skalanya ke sistem
kontinu.

Kata kunci: lumpur anoda, perolehan perak, ekstraksi perak, proses klorinasi

Received: 28 February 2017, first revision: 14 March 2017, second revision: 17 April 2017, accepted: 27 April 2017. 31
 INDONESIAN MINING JOURNAL Vol. 20, No. 1, April 2017 : 31 - 38

INTRODUCTION silver can be separated from the slime after

extracting the copper. His research was
Anode slime is a byproduct of copper reinforced by Aktas (2010) who studied silver
electrorefining process. It contains copper, recovery from spent silver oxide button cell.
lead, gold, silver, selenium, tellurium, arsenic, Silver is selectively precipitated as silver
nickel, platinum, silica and other elements. In chloride using potassium chloride solution,
processing anode slime, extraction of ensuring that other impurities remain in the
precious metals becomes the main object, solution. Silver chloride is subsequently
especially gold, silver, selenium, tellurium, reacted with metallic zinc powder in 1.0 M
and platinum. At the first stage, the study HCl to yield metallic silver of 99.99% purity.
usually separates base metals content such Extraction of silver has already patented in
as copper and lead into concentrate valuable the US Patent 3658510 A (Ernst Runyon G
elements. Gold and silver are then extracted and E, 1972). In this study, the anode slime
followed by other precious metals. was dissolved in hydrochloric acid to produce
silver chloride that could be separated from
Separating the precious metals from anode other metals. Wang et al. (1981) were
slime has been conducted commercially. recovered precious metals such as gold,
According to Chen et al. (2015), the existing silver, selenium, tellurium etc. from anode
processes of anode slimes include slime by the hydrometallurgical process. It is
pyrometallurgy (auto tech process), mentioned that to anode slime should be first
hydrometallurgy (Hoffman process) and hybrid leached by nitric acid at an elevated
processes that combine pyrometallurgy and temperature in terms of obtaining a leach
hydrometallurgy technologies. The three solution with 95% by weight of silver. The
technologies are based on the form and leachate silver nitric was then recovered in
characteristics of silver and gold-copper anode the form of silver chloride.
slimes. However, many researchers are still
searching alternatives for the more economical In contrast, the anode slime of PT Smelting
route. Many different solvents have been used Gresik commonly contains high lead, but
such as sulphuric, chloride as well as nitric another copper refining contains high copper.
acids to separate the base metals which are In this case, the copper should be separated
dominated the anode slimes, then it follows by before the precious metals as performed by
precious metals extraction. The study of silver Kilic, Kartal and Timur (2013). The anode
extraction is a continuation of the previous slime was dissolved in sulfuric acid to
studies (Rodliyah et al., 2011, 2013) to seek a separate copper. Selenium was then leached
new method using safer reagents, lower in sodium hydroxide. The recovery had
energy requirement and low investment as reached 94% copper and 86.8% selenium.
well as low operation cost. Other studies that are also conducted by
Backstrom (2010) and Wang, Wesstrom and
Hydrometallurgical processing of anode slime Fernandez (2003) to extract precious metals
from the refining of soldering scrap had been such as selenium and tellurium of anode
conducted by Harangi, Kulcsar and Kekesi slime which contains copper and nickel. In
(2015) in two steps. The first stage was pressure oxidation leaching of copper anode
leaching the anode slime by hydrochloric acid slimes, more than 65% of the tellurium is co-
to remove the tin component. As silver is extracted during decopperizing. About 10 –
practically not dissolved in this nitric acid, tin 15% of the selenium is also dissolved
can be leached from the residue by such a simultaneously by oxidation leach conditions.
medium. Copper, which was not dissolved in
the hydrochloric acid leaching step may also Researchers also extracted precious metals
follow silver. Precious metals extraction had from electronic waste as accomplished by
been accomplished by many researchers. Bigum, Brogaard and Christensen (2012). It
(Hait et al., 2002; Hait, Jana and Sanyal, is mentioned that the silver, gold, palladium
2009) published a review of anode slime and other metals could be extracted. Chen
processing, including anode slime leaching and Dutrizac (2004) examined gold
by sulfuric acid. Research on gold, silver and separation from anode slime. It was that
copper separation had been accomplished by some of the gold was available as tiny
Bard and Sobral (2008) using hydrochloric metallic gold particles. The gold was
acid solution adding sodium hypochlorite associated with selenide particles that were
solutions as an oxidizing agent. The gold and soluble in the electrolyte of sulfuric acid due

32
 Extracting Silver from Anode Slime After Lead and Gold Separations, Isyatun Rodliyah and Siti Rochani

to the presence of chloride and thiourea. The procedure above. The flow diagram is
copper separation will generate Ag-Au shown in Figure1.
selenide phase that is rich in gold and silver.
Furtherly those elements can be separated.
RESULTS AND DISCUSSIONS
As mentioned above, many typical routes of
silver extraction from anode slimes have Elemental composition of metals in anode
been determined by previous researchers. slime can be seen in Table 1. The table
However, this paper only discusses the shows that lead has the highest content
different process for extracting silver from (63.90%). Consequently, such a metal needs
anode slime through lead separation, to be separated by dissolving it in an
followed by gold separation and continued by ammonia solution to get the valuable metals
leaching with ammonia to produce the silver. from the slime (Rodliyah et al., 2011). The
The dechlorinated and chlorinated gold second highest element content is selenium
separating residues had been used as (4.97%), followed by silver (4.25%). Selenium
samples for the silver extraction to get the is valuable when it is extracted from the
highest extraction recovery. anode slime. Other valuable elements such
as gold have been extracted by Rodliyah et
al. (2013) with the recovery of 99.99%.
METHODOLOGY

In this study, the silver was separated from Table 1. Composition of anode slime
chlorination residues from anode slime after
lead separation (Rodliyah et al., 2011, Element Content
2013). The extraction process is divided into Gold (Au) 0.924 %
two types namely: Silver (Ag) 4.25%
- chlorination residue was leached by Platinum (Pt) 7.65 ppm
Palladium (Pd) 40 ppm
ammonia at varying concentrations of 1, Selenium (Se) 4.97%
3, 5 and 7 M; and dissolution Lead (Pb) 63.9%
temperatures of 30, 40 and 60 °C. The Tellurium (Te) 101 ppm
leaching residue was filtered and washed Copper (Cu) 0.28%
with dilute ammonia and the silver chloride Iron (Fe) 0.02%
was then evaporated by heating or
blowing it with hot steam to diminish
residual ammonia. The silver chloride was Due to very high lead concentration in anode
then dissolved in 6-M hot hydrochloric slime, extracting the lead will increase the
acid. A small amount of hydrogen concentration of the valuable element as
peroxide was added into the material just analyzed by Atomic Absorption Spectrometry
before the end of the dissolution process. method and is shown in Table 2. The silver
After that, deionized water was added to increases from 4.25 to 8.10%, while the lead
precipitate the silver chloride and then decreases from 63.90 to 22.00%. However,
heated at 100 °C along with strong the lead is still high and could be further
stirring. The next stage was adding separated by dechlorination process using
sodium hydroxide to form silver oxide as sodium carbonate.
well as supplementing dextrose or other
reducing sugar to the slurry in terms of
reducing silver oxide to metallic silver. Table 2. Results of AAS analysis for lead
This process took about 15 to 60 minutes. leaching residue
- chlorination residues were dechlorinated
by adding water to reach a concentration No Element Content
of 1000 g/L along with the gradual addition 1 Gold (Au) 1.61%
2 Silver (Ag) 8.10%
of sodium carbonate to obtain a constant
3 Lead (Pb) 22.00%
pH then it was filtered. The residue was 4 Platina (Pt) 11 ppm
washed by nitric acid to achieve pH 5 and 5 Palladium (Pd) 77 ppm
was cleaned by water. The residue was
ready for silver extraction using the first

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 INDONESIAN MINING JOURNAL Vol. 20, No. 1, April 2017 : 31 - 38

Figure 1. Flow diagram for silver extraction process

The XRD analysis of lead residue is shown to get recovery of 98.86% gold. The
in Table 3. The content is dominated by chlorination residues were then used for
33.94% downeyite (SeO2), 8.9% native extracting the silver. XRF analysis of
selenium (Se) and other silver minerals such chlorination residue shows more valuable
as 6.67% pavonite (AgBi3S5), 6.22% elements (Table 4). It seems that the silver
acanthite (Ag2S) and 5.42% fischesserite content reaches to 18.27%. It significantly
(Ag3AuSe2). This result shows that the increases compare to the lead residues
residue contains mostly silver and selenium. (Table 2). However, the lead slightly
increases to 54.43%. Selenium content
The 1.61%-gold (Table 2) facilitates gold reaches to 1.63%. Such condition shows
extraction by wet chlorination process. The that the residue is ready for silver and
experiment was performed by adding NaOCl selenium extraction.

34
 Extracting Silver from Anode Slime After Lead and Gold Separations, Isyatun Rodliyah and Siti Rochani

Table 3. Results of XRD analysis for lead The silver chloride is then dissolved in 6M
leaching residue hot hydrochloric acid and a small amount of
hydrogen peroxide is added just before the
Content, end of the dissolution process. At a
No. Mineral Formula
(%) concentration of 6-M hydrochloric acid, the
1 Anglesite PbSO4 1.61 chlorine gas can immediately be liberated
2 Fischesserite Ag3AuSe2 5.42
3 Selenium Se 8.18
and would tie up any gold or platinum group
4 Rooseveltite BiAsO4 2.87 metals that might exist within silver chloride
5 Pavonite AgBi3S5 6.67 deposit. Leaching silver chloride is intended
6 Bismite Bi2O3 2.10 to separate the impurities elements that
7 Acanthite Ag2S 6.22 might be carried along with silver chloride
8 Downeyite SeO2 33.94 and activated the silver chloride crystals
hence the silver can react faster over the
next reduction step.
Table 4. Results of XRF analysis for
chlorination residue Deionized water is added to precipitate
silver chloride and heated at 100 °C along
Content, with intense stirring. The next step, sodium
No. Compound/element Formula
%
hydroxide is added to form silver hydroxide
1 Gold Au 0.47
and then is dehydrated into silver oxide,
2 Silver Ag 18.27
3 Lead Pb 54.43 following such a reaction:
4 Platinum Pt < 0.01
5 Palladium Pd < 0.01 AgCl + NaOH → NaCl + AgOH ................. (3)
6 Selenium Se 1.63
7 Arsenic oxide As2O3 < 0.01 2AgOH → Ag2O + H2O .............................. (4)
8 Bismuth oxide Bi2O3 < 0.01
9 Rubidium oxide Rb2O < 0.01 Dextrose or other reducing sugar is added to
10 Antimony oxide Sb2O3 <0.01 the slurry to reduce the silver oxide into
11 Silicon dioxide SiO2 0.92
metallic silver. This reduction process occurs
12 Tin dioxide TiO2 0.28
13 Tellurium oxide TeO 0.15 about 15 to 60 minutes through the reaction:
14 Zinc oxide ZnO 0.01
15 Chromium dioxide Cr2O 0.04 12Ag2O + C6H12O6 → 6CO2 + 6H2O + 24Ag (5)
16 Copper oxide CuO 0.04
17 Nickel oxide NiO 0.02 Reactions (1) – (5) proved that the
18 Magnesium oxide MgO 0.40 conducted experiments can extract silver
from chlorination residue. The experiments
were conducted by varying ammonia
Silver Extraction from Chlorination concentration and at different leaching time
Residue (15, 30, 45 and 60 minutes), temperature
(30°C), stirring speed (100 rpm) and % solid
Lead and gold separation yield silver (20). The result is shown in Figure 3.
containing residue that can be extracted for
its silver using ammonium hydroxide Figure 2 shows the extracted silver and lead
solution. This process takes less than an contents. It can be seen that after gold and
hour. Its reaction is as follow: lead separation, chlorination residue
contains mostly silver chloride (AgCl) and a
2NH4OH → AgCl + (Ag (NH3) 2+) + Cl + little amount of lead chloride (PbCl2). The
2H2O .......................................................... (1) experiment shows that the percentage of
extracted silver increases with higher
The leaching slurry is then filtered and concentrations of ammonium hydroxide as
washed by dilute ammonia to release well as leaching time. In relation to
soluble silver salts from the slurry. Silver ammonium hydroxide concentration of 5M
chloride is then heated or blown by hot and 7M, the silver extraction percentage is
steam to evaporate remaining ammonia. almost equal than that of the next trial that
Evaporation reaction is: was set to the concentration of 5 M.

[Ag (NH3) 2] Cl → AgCl + 2NH3 ................. (2)

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 INDONESIAN MINING JOURNAL Vol. 20, No. 1, April 2017 : 31 - 38

60 heating experiment at 30°C is enough.

55 However, increasing the temperature up to
Extraction persentage
50
45 40°C and 50°C would boil the solvent faster
40 and decrease its ability to leach the silver
35
(%)

30 from the residue. The best leaching time is

25
20 60 minutes as shown in Figure 3.
15
10
5 Considering the percentage of silver
0 extraction that did not satisfy (only 53.56%)
0 5 10 15 20 25 30 35 40 45 50 55 60 65 70
results in requiring more trials. It is assumed
Time (minutes) that the available chlorides within residue
% Ag 2M % Ag 3M % Ag 5M have blocked the solvent to extract the
silver. However, dechlorination process prior
% Ag 7M % Pb 2M % Pb 3M
to the residue should be accomplished.
% Pb 5M % Pb 7M
Silver Extraction from Chlorination
Residue Through Dechlorination Process
Figure 2. Silver extractions with varying
concentrations (temperature = 30 °C, stirring As mentioned earlier that in silver extraction,
speed = 100 rpm and % solid = 20) silver and lead occurs in the form of silver
chloride (AgCl) and lead chloride (PbCl2).
Both of them are a solid form. Thus they
The next experiments were conducted to remain within residue. To obtain optimum
determine the effect of temperature on silver solubility of the silver, dechlorination of
leaching. The result of the experiment can residues is required namely by adding
be seen in Figure 3. sodium carbonate to form Ag-ammonium
complex. Its solubility decreases rapidly with
increasing concentration of chloride ion-free.
60
Extraction percentage

55 At first dechlorination process was

50
45 accomplished by mixing chlorination residue
40
35 within water with sodium carbonate
30
(%)

25 gradually, to obtain a constant pH. The

20
15 purpose of mixing residue Na2CO3 is to get
10
5 a concentration around 1000g/L. This
0
0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 reaction is easy to be controlled by
measuring the slurry pH through the sodium
Time (minutes)
carbonate addition. The amount of required
sodium carbonate can be estimated from its
% Ag 30C % Ag 40C % Ag 50C
reaction stoichiometry between the lead
% Pb 30C % Pb 40C % Pb 50C chloride and the sodium carbonate. The
reaction of the process is:

Figure 3. Extracted silver yielded from different PbCl2 + Na2CO3 → PbCO3 + 2NaCl .......... (6)
temperatures and leaching times (NH4OH
concentrations: 5 M, stirring speed: 100 rpm The lead sulfate within residue might also be
and % solid: 20)
carbonized as shown in reaction:

PbSO4 + Na2CO3 → PbCO3 + Na2SO4 ..... (7)

It is assumed that that ammonia is the
cause. It can be seen that if the leaching
During the process, hydrocerussite [Pb3
temperature increases, the percentage
(CO3)2(OH)2] might also be formed as shown
extracted silver decreases. It is assumed
in reaction as follows:
that ammonia evaporation is the cause, thus
the ability of ammonium hydroxide in silver
3PbSO4 + 3Na2CO3 + H2O → [Pb3
leaching from the residue declined.
(CO3)2(OH)2] + 3Na2SO4 + CO2 ................ (8)
Ammonium hydroxide itself has a boiling
temperature around 27°C; therefore the

36
 Extracting Silver from Anode Slime After Lead and Gold Separations, Isyatun Rodliyah and Siti Rochani

The difference of PbCl2 and PbSO4 solubility be scaled up as well as conducted to a

compared to that of PbCO3 is significant. continuous system.
Thus, conversion of PbCl2 and PbSO4 to
form PbCO3 can completely take place.
AgCl is less soluble than Ag2CO3, therefore, ACKNOWLEDGEMENTS
AgCl is unaffected by sodium carbonate
leaching. Dechlorination process is intended The authors would like to acknowledge PT
mainly to separate the lead, thus the silver in Smelting Gresik for supplying the anode
the residue becomes more concentrated slime for the research. The authors would
and does not interrupt the extraction also like to show appreciation to the Ministry
process. of Energy and Mineral Resources for
research funding and also colleagues who
After lead separation, further experiments is involved in conducting the research.
silver extraction using 5-M ammonium
hydroxide and leached for 60 minutes, at
30°C. As expected, silver recovery increased REFERENCES
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