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Hydrometallurgy 92 (2008) 48 – 53
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Acid dissolution of alumina from waste aluminium dross

B. Dash a , B.R. Das a , B.C. Tripathy a,b,⁎, I.N. Bhattacharya a , S.C. Das a
a
Institute of Minerals and Materials Technology (CSIR), Bhubaneswar-751 013, India
b
Hydrometallurgy Division, MINTEK, 200 Hans Strijdom Drive, Randburg, South Africa

Received 13 August 2007; received in revised form 7 January 2008; accepted 15 January 2008
Available online 26 January 2008

Abstract

Aluminium and its chemicals are generally produced from its oxidic ores, mainly bauxite through NaOH leaching by Bayer's process. There
are other oxidic raw materials such as coal ash, clay etc. which are being explored with little success.
Aluminium dross formed while melting of aluminium in presence of air is recycled back to the smelter to recover the residual aluminium after
salt treatment. The remaining residue dross is usually considered as a waste. This contains a complex mixture of mostly aluminium oxide (50–
75%), remaining metallic aluminium, nitride, carbide and sulphide of aluminium, some alloying elements and salts. On one hand, this residue is
considered as hazardous waste, on the other hand as a rich source of alumina.
In the present study the waste dross rich in alumina value was taken for acid dissolution studies to recover alumina value. The material
responded favourably towards the acid dissolution. The washed material under stoichiometric condition of acid leached out ∼85% of alumina
while under stringent condition more than 90% could be leached out. The results obtained therefore, shows that aluminium dross could be utilized
to prepare alumina chemicals and thereby avoiding stockpiling.
© 2008 Elsevier B.V. All rights reserved.

Keywords: Aluminum dross; Alumina; Sulphuric acid; Dissolution; Characterization; Waste utilisation

1. Introduction
Aluminium and its chemicals are produced mainly from
bauxite an oxidic ore, through alkali leaching by Bayer's
process. At the same time many investigators have also tried to
modify the Bayer's process (Filippou and Paspaliaris, 1993;
Dash et al., 2007) as well as to utilize raw materials other than
the bauxite ore (Hector et al., 1997). Mostly clay has been
considered as an alternative to bauxite and has been tried by
both alkaline and acidic routes to see its feasibility. For treating
clay in acidic route it is first roasted at around 1000 K. It
changes the kaolinite to meta-kaolin from which the aluminium
can be dissolved as acid salt. US bureau of mines along with
some aluminium companies made an effort to investigate acid
processes from clay (Habashi, 1997). For several reasons the
hydrochloric acid process was preferred. Pachiney and Alcoa
⁎ Corresponding author. Institute of Minerals and Materials Technology
(CSIR), Bhubaneswar-751 013, India.
0304-386X/$ - see front matter © 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.hydromet.2008.01.006
jointly operated a pilot plant where the leachant was a mixture
of HCl and H2SO4 (Habashi, 1997). The combination of acids
eliminated the need to roast the clay. Other processes use
H2SO4, H2SO3, HNO3 or NH4HSO4 as reagents. Clay is a major
impurity of coal, so the ash from coal may be considered as
over-roasted clay. Acid processes applied for clay can be used to
extract alumina from coal ash with minor modifications
(Habashi, 1997). Several investigations have been undertaken
to extract alumina from coal based feed materials and in
particular the extraction of aluminium from kaolinite, illite and a
number of colliery spoils and coal ash materials (Habashi,
1997).
Kelmers et al. (1982) reviewed the chemistry of the direct
acid leach, calsinter and pressure digestion-acid leach methods
for the recovery of alumina from fly ash. As a conclusion, alu-
minium dissolution depends on the solid phases present, which
are related to the basic element content of the ash.
It was observed that the rate of extraction of aluminum
from clay based materials in mineral acid leaching systems is
strongly dependent on the thermal history of the feed materials
 B. Dash et al. / Hydrometallurgy 92 (2008) 48–53
(Livingston et al., 1983a,b), which were classified into 3 cate-
gories, such as:
i) Uncalcined material and material calcined below 823 K
(relatively low yield of Al2O3 with mineral acid leaching).
ii) Materials calcined between 823 and 1123 K (high yields).
iii) Materials calcined beyond 1123 K like coal and clay
based materials (very low yield).
Though the reason of this behaviour is not clearly under-
stood, the transition temperature is related to temperature of
phase changes, dehydroxylation and lattice destruction reaction.
The majority of the proposed routes for recovery of alumina
from clay based materials involve the acid leaching of feed
materials which have been calcined under controlled conditions
in the temperature range between 823 and 1123 K (Christie and
Derry, 1976). Bailey and Chapman (1987) studied the effect of
fluoride ions on the HCl leaching of clay based material like
kaolinite and a number of colliery spoils and coal ash materials.
Aglietti et al. (1987) reported leaching of north eastern red soil
with 6M HCl to extract alumina.
Phillips and Wills (1982) studied Al2O3 recovery from china
clay micaceous residue using HNO3 and found that maximum
alumina recovery was achieved with re-calcined feed material.
Similarly dissolution of alumina from high silica power station
fuel ash using dilute H2SO4 has been reported by Verban and
Louw (1989).
According to Torma (1983) and Freeman (1993) coal ash
could be an important source of pre-mined minerals, particularly
alumina, which is presently extracted from bauxite resources.
Though HCl and HNO3 leaching of alumina and other minerals
have been developed, the processes were found to be of little
practical importance due to the corrosive nature of their solutions
(Freeman, 1993).
In a study on the mechanism and kinetics of aluminium and
iron recovery from coal ash by H2SO4 treatment, Seidel and
Zimmels (1998) suggested that the leaching process involves a rate
controlling step of mass transfer. In a recent publication, Matjie
et al. (2005) attempted to extract aluminium from a South African
Fig. 1. XRD pattern of aluminium dross of particle size finer than 850 μm (Tyler 20).
49
mullite containing coal ash by calcining with calcium oxide at a
temperature of 1273–1473 K followed by leaching with H2SO4
which resulted in an extraction efficiency of 85%. The forgoing
discussion on acid leaching of aluminium containing raw materials
other than bauxite ore such as clay or clay based feed materials like
coal or fly ash was made to focus on the behaviour of these oxidic
materials of aluminium towards acid leaching. As discussed
above, clay or coal requires heat treatment for effective dissolution
of alumina. Aluminium can be extracted efficiently only when clay
is pre-roasted at ∼1000 K prior to acid treatment. Similarly coal/
fly ash treated in the range of ∼800 and 1100 K followed by acid
leaching yields more than 80% alumina dissolution.
Aluminium dross, a complex oxidic material, is formed when
molten aluminium comes in contact with air at the outer surface
of the melt. This primary dross is generally recycled back to the
smelter to recover the residual aluminium metal by remelting
it with salt flux to minimize oxidation. In some cases various
alloying elements are also used along with the salt flux to produce
aluminium alloy, while the remaining residue sometimes also
called as alloy dross or secondary dross is considered as a
hazardous waste material. The oxide in the dross exhibits the form
of a long continuous network where metallic aluminium stays
entrapped. The molten flux breaks this framework and facilitates
the coalescence of aluminium drops that sinks to the aluminium
bath (Livingston et al., 1983a,b; Matjie et al., 2005; Tenorio and
Espinosa, 2002). In majority of the cases, salt bath is used to
maximize the recovery of aluminium, which also helps to reduce
the impurity levels in the aluminium. By this process though
oxide generation is less, the dross becomes hazardous because of
its content which makes the disposal of residues and recovery of
alumina more complex. The increasing demand of valuable
materials and environmental standard enforcement has forced to
develop a suitable method for extracting alumina from the waste
dross.
As pointed out above, aluminium dross is formed during
aluminium melting due to aerial oxidation. Thus acid leaching
of these materials is expected to behave in a similar way to those
of coal or fly ash. In secondary aluminium dross the amount of
Al2O3 available is in the range of 50 to 75%, turning it to be the
50 B. Dash et al. / Hydrometallurgy 92 (2008) 48–53
Fig. 2. Dissolution of alumina as a function of acid volume at different
percentage of H2SO4 concentration, dross 10 g.
richest alumina source. A survey in USA (Kulik and Daley,
1990) showed generation of dross was around 800 000 tons in
1988 which has increased since then at the rate of 3 to 4% each
year. A rough estimate shows that about 75 000 tons of dross is
generated in India each year.
Scanty literature is available on the alloy dross (secondary
dross) treatment. Attempts have been made to extract alumina
from the alloy dross by adopting either pyro- or hydro-
metallurgical methods (Tenorio and Espinosa, 2002; Kulik and
Daley, 1990; Zuck, 1995; Lavoie and Lachance, 1995; Lavoie
et al., 1991; Kemeny et al., 1992; Park et al., 1999; El-Katatny
et al., 2003; Osborne, 1995; Garret, 1982; Huckabay, 1984;
Huckabay and Skiathan, 1984; Durward and Arthur, 1982;
Amer, 2002). In the hydro-metallurgical method the metal is
either recovered by dissolving the dross in alkali (Kemeny et al.,
1992; Park et al., 1999) or H2SO4 media (El-Katatny et al., 2003;
Osborne, 1995; Garret, 1982; Huckabay, 1984; Huckabay and
Skiathan, 1984; Durward and Arthur, 1982). The findings of
most of these studies are patented and details are not available.
Amer (2002) carried out the dissolution of waste dross in two
steps. In the first step dilute sulphuric acid (5–12.5%) was used to
leach out the impurities and in the second step concentrated acid
(30–40%) was used to extract Al2O3 in pure state. In this case, the
required amount of acid was mixed with the purified dross
obtained after the first step and a homogeneous paste was made,
which was then heated in a furnace. The heated mass was then
boiled with water to dissolve the anhydrous aluminium sulphate.
Fig. 3. Dissolution of alumina as a function of solid concentration at different
acid concentrations.
Fig. 4. Dissolution of alumina with different acid concentrations, dross 10 g.
Similarly Miskufova (2005) also studied the dissolution of dross
using sulphuric acid. In both the above investigations (Amer,
2002; Miskufova, 2005) attempt was made to produce aluminium
sulphate from the waste dross.
However in the present study detailed dissolution behaviour
of the waste dross has been studied in sulphuric acid to find out
the best condition for maximum recovery of alumina from the
waste dross confirming it to be a rich source of aluminium and
avoiding stockpiling.
2. Materials and methods
Secondary aluminium dross is a waste material obtained from aluminium
melting plants whose composition differs due to the various alloying elements used
during remelting of the primary dross. The dross used in this work was collected
from a domestic dross producer, which contains mainly around 65% alumina, 4%
SiO2 and oxides of Mg, Ca and Fe along with some salts such as NaCl and KCl.
This dross contains larger particles of 2–5 mm in size, which are mostly metallic
aluminium or its alloys and the finer fractions are mostly alumina (Al2O3).
Screening of the above material was undertaken to separate out the aluminium and
the alloy part from the oxide. Thus the finer particles of size finer than 850 μm
(Tyler 20) were only taken for the present study. Philips X-ray Fluorescence (XRF)
analytical equipment was used for dross analysis. The X-ray Diffraction (XRD)
analysis was carried out on a Philips Powder diffractometer Model PW 1830 X'pert
system. Carbon and sulphur were analysed by a LECO instrument.
The experiments on the dissolution of dross in H2SO4 were carried out in a
flat-bottomed glass reactor, which was placed on a Remi make hot plate cum
magnetic stirrer and temperature was maintained at 90 ± 2 °C. The dissolution
reaction is exothermic and the slurry attains a temperature of 80 ± 5 °C without
Fig. 5. Dissolution of alumina as a function of time and different acid
concentrations.
 B. Dash et al. / Hydrometallurgy 92 (2008) 48–53
Fig. 6. Dissolution of alumina with acid concentration for washed and original
dross, dross 10 g.
any input of heat from out side. In each case 10 g of dross was taken unless
otherwise specified. Each experiment was carried out for 3 h and then the leach
liquor was analysed by conventional EDTA–ZnSO4 method (Vogel, 1961) to
determine the amount of alumina extracted. All the experiments were carried out
in duplicate and the average values were taken.
3. Results and discussion
3.1. Characterisation of alumina
The alumina generated during melting of aluminium has been
characterized by many investigators (Park et al., 1999; Miskufova,
2005; Stewart, 2003; Maason and Taghiei, 1989). Park et al. (1999)
have reported that the main phases present in the Korean dross are α-
Al2O3, metallic aluminium and MgAl2O4. Miskufova (2005) reported
that the major constituents are AlN, Al2O3, NaCl, MgO.Al2O3 and
minorities are Al, KCl, Si, SiO2, kryolite, carbide of aluminium,
some chlorides and fluorides. Similarly, Stewart (2003) suggested that
dross contains Al2O3, AlN, AlC, MgF2, NaAlCl4, KAlCl4, SiO2, MgO,
MgO.Al2O3 and the salt constituents. But according to Maason and
Taghiei (1989), besides above compounds it also contains some
intermediate phase composed of KMgF3 or K2NaAlF6.
Fig. 7. XRD pattern of acid leached residue.
51
In the present study the finer particles (b850 μm) taken for the
dissolution study were subjected to chemical and X-ray Diffraction
(XRD) analyses. Fig. 1 shows the typical XRD pattern and the various
phases present in the dross under study.
The chemical analyses indicated that the dross contains: Al2O3: 64.8,
CaO: 0.93, SiO2: 4.0, Fe2O3: 1.5, MgO: 3.2, Na2O: 2.75, K2O: 0.51, Cl:
3.9, C: 1.25, S: 0.22% and LOI: 14%. The XRF and X-ray diffraction
analyses confirmed the presence of α-Al2O3, CaF2, metallic aluminium,
MgAl2O4, Fe2O3, CaO, carbon, sulfur and salts like KCl and NaCl.
3.2. Acid dissolution
Dissolution of alumina in sulphuric acid seems to be quite interesting
and complex in nature too. Increase in proton activity i.e. acidity will
render higher dissolution; however, increase in sulphate ion concentration
i.e. sulphuric acid will decrease the rate of dissolution due to the precipi-
tation of aluminium sulphate. Thus a compromise between acidity and
sulphate ion concentration has to be established in the solution to ensure
efficient dissolution of alumina from the dross in sulphuric acid solution
avoiding precipitation. Therefore, dissolution of alumina depends on the
availability of both acid as well as water in the acid solution for keeping
the aluminium sulphate dissolved during dissolution process.
To evaluate the behaviour of alumina dissolution, 10 g of dross was
subjected to leaching with increasing amount of acid (36N) at two
different percentages of acid concentration (20% & 40%, v/v). In this
the acid amount was varied from 15 mL to 50 mL in such a way that the
percentage of acid is kept constant such as 20% or 40%. Therefore with
increase in acid amount the amount of water is increased to keep the %
acid constant to 20% or 40%. The results are shown in Fig. 2. It may be
seen that nearly 75% of alumina dissolves when dross is leached with
20 mL of acid at 20% acid concentration. By increasing the acid volume
to 30 mL, the efficiency increased to around 80% but it remained almost
constant beyond this. An increase in acid concentration to 40% also
produced similar trend in alumina dissolution. But in this case maxi-
mum efficiency obtained is around 86% at 40 mL of acid quantity and
thereafter the efficiency remained almost constant with increase in acid
quantity. It may be noted that for all these acid concentrations, with
increase in the volume of acid the efficiency initially increases and then
remains constant beyond certain quantity. It has been further found that
initially at the same acid amount the recoveries are less for higher
concentrations of acid (40%) than the diluted acid (20%), and at 30 mL
of acid amount in both the cases recovery is same, but the recovery
52 B. Dash et al. / Hydrometallurgy 92 (2008) 48–53
overtakes in concentrated acid when acid quantity is increased beyond
30 mL. The low recovery with concentrated acid at lower amount may
be due to the availability of less water for dissolution of aluminium
sulphate which is formed during the reaction.
Thus it has been observed that concentrated acid requires more water
for dissolving the aluminium sulphate, even when percentage of acid is
kept the same. For lower concentration of acid an increase in the volume
of acid does not have much impact on dissolution. Therefore at each level
of acid concentration optimum quantity of acid and water are important. It
should be noted that 15 mL acid is sufficient to dissolve 10 g of aluminium
dross based on stoichiometry. From this behaviour it seems the dissolution
kinetics and solubility of aluminium sulphate formed are fully dependent
on the amount of both acid as well as water present in the leachant.
Fig. 3 shows the dissolution behaviour of dross oxide with 25, 30
and 40% acids with variation of solid concentration. In all three cases
the leaching efficiency initially increases, reaches a maximum and then
falls. The dissolution is maximum around a solid concentration of 10%.
Fig. 4 shows alumina dissolution behaviour with acid concentration
in the leachant using 10% solid. A sharp increase in dissolution takes
place when sulphuric acid concentration is raised from ∼ 10% to 30%,
where a maximum recovery of ∼ 88% Aluminium is achieved. It then
followed a slow fall up to 50% acid from which a rapid fall in the
dissolution of alumina is observed. The decrease in aluminium
recovery at 70% acid may be due to lower solubility of aluminium
sulphate in concentrated acid. The results indicated that around 85%
alumina can be dissolved in the acid within the range of ∼ 25–50%
sulphuric acid. As discussed above an optimum quantity of acid and
water is absolutely required for effective dissolution of alumina.
The dependence of dissolution reaction on the time was studied
using acid concentration in three different levels (Fig. 5). As observed
from Fig. 5, the reaction is very fast initially and within 10–15 min
nearly 60–70% of alumina dissolves. Beyond this the rate of reaction is
slow, probably due to formation and coverage of the surface of the dross
particle by either basic aluminium sulphate or aluminium sulphate,
depending on the amount of acid present in the leachant. However, the
reaction continues and reaches maximum by 60 min after which
dissolution is almost nil. This implies that the dissolution of alumina
may be carried out for 60 min only for achieving optimum dissolution.
3.3. Salt effect on alumina dissolution
It has been mentioned earlier in Section 2, that waste aluminium
dross also contain salts like KCl and NaCl. The chemical analysis
shows a salt content of about 8%. Thus, during the sulphuric acid
dissolution, these salts must have dissolved into the leach solution and
might have some effect on the dissolution reaction rate.
In order to evaluate the salt effect, the oxide was made salt free by
repeated hot water washing and then taken for dissolution. Fig. 6 shows the
dissolution behaviour of both original dross oxide and the salt free oxide.
A significant change in the dissolution behaviour is observed when
the oxide is made salt free. With 15% acid, about 85% dissolution takes
place with salt free oxide whereas at the same condition only ∼ 70%
dissolution takes place with the original dross oxide. The difference in
dissolution between washed & non-washed dross oxide is more
significant at lower levels of acid concentrations. But increasing the
acid concentration to 30%, dissolution increases by 6–7% in both the
cases. However further increase in the concentration of the acid,
increased the leaching efficiency of the salt free oxide to ∼ 95%. On the
other hand, it did not show any further enhancement in leaching
efficiency with the original non-washed dross oxide.
The remaining residue after acid leaching was subjected to X-Ray
diffraction analysis (Fig. 7). The results showed that the residue
contains aluminium mainly as α-Al2O3, and MgO.Al2O3. Perhaps, the
residue might have some more compounds such as silimanite in trace
amount, which could not be traced from X-ray diffractogram. These
compounds remained undissolved under the present conditions and
may require more stringent leaching conditions. The graphite phase has
intensified compared to the original dross indicating as the major phase
present in the acid leached residue dross.
4. Conclusions
• It is possible to recover aluminium from secondary alloy
dross almost completely without any pre-treatment by
leaching in sulphuric acid.
• For effective dissolution, not only higher acid amounts are
required but also substantial amount of water must be in the
leachant for keeping the aluminium sulphate in dissolved
condition, thus facilitating the reaction to proceed.
• Maximum dissolution is possible at an optimum concentra-
tion of acid and water.
• Even without pre-treatment, more than 85% of alumina dis-
solves under the conditions: 30% H2SO4, 10% solid concen-
tration, 90 °C and dissolution time of 1 h.
• The salts present in the dross are found to affect the be-
haviour of dissolution process. After removal of these salts it
is possible to dissolve nearly 85% of alumina with 15% acid.
However increasing the acid concentration to 50% increased
the alumina dissolution further to ∼ 95%.
Acknowledgements
The authors are grateful to the Ministry of Environment and
Forests, Govt. of India, New Delhi, for the financial support to
carry out this work. They are also grateful to M/s Agarvanshi
Aluminium, Secunderabad for supplying the aluminium dross.
The authors also like to thank the Director, Institute of Minerals
and Materials Technology, for permission to publish this paper.
They are also thankful to Dr. P.S. Mukherjee and Dr. Rajeev for
the XRD and XRF analyses.
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