Minerals Engineering 19 (2006) 140146

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An investigation into the feasibility of recovering

valuable metals from solid oxide compounds by gas phase
extraction in a uidised bed
J.H. Potgieter a,*, M.A. Kabemba b, A. Teodorovic c,
S.S. Potgieter-Vermaak a, W.G. Augustyn d
a
School of Chemical and Metallurgical Engineering, University of Witwatersrand, C/o Jan Smuts Avenue and Empire Road,
Braamfontein Johannesburg, Johannesburg, Gauteng 2000, South Africa
b
Department of Chemical and Metallurgical Engineering, Tshwane University of Technology, South Africa
c
Faculty of Science, University of Kragujevac, YU 3400, Serbia and Montenegro
d
Department of Chemistry and Physics, Tshwane University of Technology, South Africa

Received 28 June 2005; accepted 12 August 2005

Available online 27 September 2005

Abstract

Recent years have seen the application of the concept of uidisation extended to dierent kinds of industrial processes. This technol-
ogy now plays a central role in the chemical and petrochemical industries, in power generation and in mineral processing and metallurgy.
The current research is directed towards gas-phase extraction of metals because of the high yield of recovery that can potentially be
achieved. This process achieves the extraction of metals by using a volatile organic reagent, which passes through the feed material
and reacts selectively with the metal to be extracted. The product is a volatile metal complex, which is removed from the residual gangue
by a carrier gas.
The results showed that the procedure could be successfully applied to recover aluminium, chromium, vanadium and iron with acet-
ylacetone from their respective solid oxides in a uidised bed. The percentage recovery ranged from 75.2% for iron to 48.2% for chro-
mium. Kinetic investigations were performed to estimate the activation energy required for each reaction. The recovery of the metals
depended on the temperature and reaction time.

2005 Elsevier Ltd. All rights reserved.

Keywords: Reaction kinetics; Oxide ores; Extractive metallurgy; Minerals processing

1. Introduction Various slags are produced as by-products in metallurgi-

Valuable metals such as chromium, aluminium, vana-
dium and iron can potentially be recovered from wastes
of the ferro-alloy industry at a cost considerably lower than
for furnace operations, by using a uidised bed technique.
The size and quality of the products render them directly
saleable, without the need for re-melting (Mintek, 1999).
*
Corresponding author. Tel.: +27 117177546; fax: +27 114031471.
E-mail address: hermanp@prme.wits.ac.za (J.H. Potgieter).
cal processes or as residues in incineration processes. Slags
usually contain a variety of valuable metals. They are actu-
ally a secondary resource of metals, rather than an end-
waste and have been applied as a resource material in many
areas (Geiseler, 1996). In addition, for some applications,
slags have comparable or even better properties than their
competitive counterpart materials. Another feature of
importance is that some slags contain a notable amount
of harmful or heavy metals. The release of these metals
may cause environment problems.
A large amount of slags is produced worldwide each
year and they usually contain a variable amount of valu-

0892-6875/$ - see front matter
2005 Elsevier Ltd. All rights reserved.
doi:10.1016/j.mineng.2005.08.002
 J.H. Potgieter et al. / Minerals Engineering 19 (2006) 140146
able metals, except blast furnace slag. By applying mineral
processing technologies, such as crushing, grinding, mag-
netic separation, otation and leaching or roasting, it is
possible to recover metals such as Fe, Cr, Cu, Al, Pb,
Zn, Co, Ni, Nb, Ta, Au, and Ag from these various slags
(Basir and Rabah, 1999).
The conventional method for disposal of slags is dump-
ing. The continued dumping of slags not only occupies
large areas of land, but also wastes resources and can have
a harmful impact on the environment due to potential
water pollution. It is therefore desirable to recover metals
from slags and utilise the slags, for example in building
or other construction applications. Several methods have
been proposed for the treatment of waste from the ferro-
alloys industry (Cohen et al., 1997; Salamon, 1995). Tradi-
tionally the recovering processes of metals can be classied
in following categories: pyrometallurgy, hydrometallurgy,
solvent extraction and ion-exchange.
Current research is now starting to focus on gas phase
extraction because of the high yield of metal recovery with
the advantage that the extractant can be continuously
regenerated (Allimann et al., 2001). This process can
achieve the extraction of heavy metal contaminants from
several matrices (low grade ore, soil, sediment, spent cata-
lysts, slags, industrials wastes, etc.) by using a volatile or-
ganic reagent, which passes through the feed material and
reacts selectively with the metal to form an extractable vol-
atile complex (Allimann et al., 2001).
A French engineer, Eugene Houdry, rst discovered and
designed a uidised solids process that has formed the
foundation of all subsequent developments in this eld
(Jehning et al., 1980). The high proportion of the elements
cited above in slag and their important use in the metallur-
gical eld led to this investigation of an alternative way of
recovering those valuable metals. This is done by treating
the materials with a b-diketone (2,4-pentanedione) as a
complexing agent, and extracting the metals through
gas phase extraction in a uidised bed reactor. All the
parameters that can usually inuence such a process,
such as temperature, total reaction time and the kinetics
of the processes were investigated and are described in this
paper.
2. Experimental
2.1. Apparatus and description of the process ow sheet
A laboratory scale glass uidised bed reactor system of
500 mm long and 15 mm in diameter was designed. The
uidised bed also contained a vessel (reactor 1) of
250 mL which carried the liquid extractant, coupled to a
tube with a coarse glass frit (reactor 2). The uidised bed
column had three outlets for thermocouples to measure
the temperature distribution in the reactor.
The product of the gas phase extraction process in the
uidised bed reactor is a volatile metal complex. It is re-
141
Carrier Gas
Extractant
(N2)
Volatilisation of extractant and
mixing with carrier gas
Extractant recycle
Gaseous Extractant
Extraction of metal
(gas-solid reaction)
Volatile extract
Recovery of
metal
Metal
Fig. 1. Process ow sheet for the vapour phase extraction of metal from
slag.
moved from the residual gangue by a carrier gas ow
and condensation (see Fig. 1). Under specic conditions,
this volatile metal complex can be reduced after condensa-
tion of the vapour phase to the metallic product and the or-
ganic reagent. The latter can then be recycled for re-use in
the process (Allimann et al., 2001). The ow sheet of the
process used is shown in Fig. 1.
2.2. Measurements
2.2.1. Preparation of the standards
Calibration standards for the UVVis spectrophotometry
analysis were prepared from synthesized metal acetylacetone
complexes (Hon et al., 1965; Earley and Cannon, 1966;
Brown, 1978; Chaudhuri and Ghosh, 1983; Stary and Hlad-
ky, 1963). Stock solutions containing 450, 2000, 1000 and
6000 mg L
1 of chromium-, aluminium-, vanadium oxy-
and ferric acetylacetone complexes, respectively were pre-
pared in absolute ethanol. Dilutions ranging from a 100
to 0.1 suced for the construction of calibration curves.
The wavelength of maximum absorbance for each com-
plex was selected by scanning a solution of the relevant
metal complex over a range of wavelengths from 200 to
800 nm. A series of standards were measured at this wave-
length to construct a calibration curve of the concentration
of the compound against its absorbance. After each exper-
iment the absorbance of the metal complex analysed was
read from the calibration curve and the concentration
determined.
2.2.2. Procedure for the recovery of metals
Reactor 2 was charged with 12 g of the relevant pure
metallic oxide (Cr2O3, Al2O3, V2O5, and Fe2O3, respec-
tively) after mixing it with 50 g of silica. Reactor 1 was
heated to a temperature (T1) of 140 C, allowing the
extractant to vaporise into reactor 2 where the reaction
with the particular oxide could occur at dierent tempera-
tures ranging from 150 C to 220 C. Each temperature was
142 J.H. Potgieter et al. / Minerals Engineering 19 (2006) 140146
maintained for a selected time, which varied from 30 to
180 min, to permit the reaction to go to completion. After
volatilisation and cooling in an ice bath, the volatile metal
complex was collected in a cold trap. The volatilised metal
complex were diluted to 250 ml with absolute ethanol and
analysed by UVVis spectrophotometry to subsequently
calculate each respective metal concentration.
2.2.3. Recovery study
All experiments were carried out in batch mode for sim-
plicity and reliability (Curckovic et al., 2001). The batch
experiments were run at dierent temperatures and reac-
tion times. The concentration of the acetylacetone, the
quantity of feed material, the gas ow rate and the mass
of silica were kept constant for each experiment to ensure
reproducibility.
The recovery for each metal was calculated from the
determined concentration. The theoretical and actual
recovery was calculated using the following equations:
Rthe C=F  100 1
Rreal Rthe  K=100 2 iation in recovery occurs when the reaction time is in-
where C is the quantity in g of the element in the extracted
solution at a given temperature and time; F is the quantity
in g of the element in the feed material; K is the coecient
of recovery when preparing the complexes (i.e. actual yield/
theoretical yield).
In this work the order of the extraction process for Al,
Cr, V and Fe was determined using kinetic models based
on chemical analogy. The integral method was used (Fog-
ler, 1986) to estimate the reaction order and integrate the
dierential equation used to model the batch system. If
the assumed order is correct, the appropriate plot (deter-
mined from this integration) of concentration-time should
be linear. This method evaluates the specic reaction rate
constant at dierent temperatures in order to determine
the activation energy. The order of the extraction process
was evaluated for rst order and second order reaction
kinetics according to the following well-known equations:
 
C0
ln kt 3
C ash using the Servo Process, which involves the extraction
1 1

kt 4 agent that is selective for the chosen metals. The dierence
C C0
where C0 is the initial concentration, C is the nal concen-
tration, k is the rate constant, t is the time in seconds.
3. Results and discussion
3.1. Recovery of aluminium
Fig. 2 shows the eect of reaction time at dierent tem-
peratures on the recovery of aluminium from the metal
oxide by forming the acetylacetone complex (Al(acac)3).
Results show that the recovery of aluminium increases with
increasing time, but reaches a maximum after about
80.0
150 C
70.0 160 C
170 C
60.0
180 C
Recovery [%]
50.0 190 C
200 C
210 C
40.0
220 C
30.0
20.0
10.0
0.0
0 50 100 150 200
Time [min]
Fig. 2. Eect of time on the recovery of aluminium at various
temperatures.
100 min. A recovery of 63.7% was achieved after 90 min
and remained at 63.7% after 105 min at temperatures of
180 C or higher. The results also show that no further var-
creased for longer than 105 min.
The extraction of aluminium also increases with increas-
ing temperature. It can be seen that the recovery improves
substantially from 160 C to 180 C when sucient time is
allowed, e.g. only 31.4% of the available aluminium is ex-
tracted after 105 min of reaction at 160 C, while 63.7%
is extracted at 180 C and 65.7% at 200 C in the same
time. The results obtained showed that an increase of tem-
perature after 180 C did not aect the recovery to any
great extent, regardless of the time allowed for extraction.
Chris et al. (2000) used thermal treatment to reduce the
metal content of y ash. This was achieved by vaporizing
the volatile aluminium from municipal solid waste
(MSW). For that reason the authors of this study used pure
Al2O3 to simulate the relevant constituent in the y ash and
found that the equilibrium time needed was longer than
90 min, as is illustrated in Fig. 2. This result concurs with
that obtained by Allimann et al. (2001). These latter
authors conducted experiments on the purication of y
of heavy metals using a volatile chelating extraction re-
in equilibrium time between their work, which was 120 min
and the values obtained in the current work, may be due to
the dierence in experimental conditions, the extractant
and the type of material used.
3.2. Recovery of chromium
The recovery of chromium increased with increasing
time and reached 48.2% after 150 min at a temperature of
at least 210 C, as is shown in Fig. 3. A further increase
in time to 150 min did not have any large eect on the
recovery process, regardless of the temperature at which
the extraction was conducted.
 J.H. Potgieter et al. / Minerals Engineering 19 (2006) 140146 143

70.0 Fig. 4 showed that the percentage recovery from V2O5 is

150 C almost constant after 120 min, regardless of the reaction
60.0
160 C temperature. At 160 C and 120 min the percentage recov-
170 C
50.0 ery is 60.9% and at 200 C for the same time it is 66%. It
180 C
Recovery [%]

190 C can also be seen that the recovery of vanadium does not de-
40.0 200 C pend on temperature to the same extent it does on time.
210 C
30.0 220 C
While the % recovery of vanadium only increases from
about 61% at 160 C to 66% at 220 C, there is an increase
20.0 of more then 50% in the percentage recovery from 30 min
10.0 to 120 min.
The results obtained here indicate that gas phase extrac-
0.0 tion of vanadium presents a viable opportunity for the
0 50 100 150 200
treatment of such wastes. The recovery of vanadium from
Time [min]
ferro-alloy waste originating from the treatment of various
Fig. 3. Eect of time on the recovery of chromium at various primary and secondary materials constitutes a challenging
temperatures. problem in the valuable metals rening industry, and the
results obtained in this investigation oer a potential way
The eect of temperature on chromium recovery by of achieving good recoveries.
acetylacetone was not as pronounced as in the case of alu-
minium. Beyond 210 C the maximum recovery seems to 3.4. Recovery of iron
stay constant with any particular reaction time employed
in the extraction process. The eect of time on the recovery of iron was studied at
The results correlate well with the work of Das et al. dierent temperatures in the range from 150 to 200 C and
(1997) who found that 180 min was needed for a recovery time intervals varying from 30 to 120 min. The results are
of 57% of chromium. Gordon and Chi-Ming (1998) studied presented in Fig. 5. It was found that the recovery of iron
the extraction ability and recovery of heavy metals by elec- with acetylacetone increases rapidly with time and reaches
trolysis from municipal incinerator y ash. Although a dif- saturation within 45 min, except at the two lowest reaction
ferent technique was used, the authors found that for temperatures. This eect can be explained by the fact that
maximum recovery of chromium to be achieved, a time iron reacts very strongly with any beta-diketone (Allimann
of 180 min were required, which is similar to the ndings et al., 2001).
of this work. Fig. 5 shows that as the temperature was raised, the
recoveries of iron improved. The maximum iron is recov-
3.3. Recovery of vanadium ered at 180 C within 45 min. Raising the temperature up
to 210 C does not improve the recoveries any further.
The eect of time on the recovery of vanadium from the Thus, 180 C seems to be the optimal temperature. During
vanadium oxide at dierent times was studied in the time the rst 30 min an almost linear increase in the percentage
range of 30180 min. The recovery of vanadium increased recovery of iron as the temperature increases, is apparent.
rapidly with time as shown in Fig. 4 and reached an opti- Extrapolation of the percentage recovery at 150 and
mum value in about 120 min. 160 C during the initial part of the reaction seems to

70.0
80.0
60.0
70.0
50.0
60.0
Recovery [%]

Recovery [%]

40.0 150 C 50.0

160 C
30.0 170 C 40.0
150 C
180 C
20.0 30.0 160 C
190 C
170 C
200 C 20.0
10.0 180 C
210 C
190 C
220 C 10.0 200 C
0.0
0 50 100 150 200 0.0
Time [min] 0 20 40 60 80 100 120 140
Time [min]
Fig. 4. Eect of time on the recovery of vanadium at various
temperatures. Fig. 5. Eect of time on the recovery of iron at various temperatures.
144 J.H. Potgieter et al. / Minerals Engineering 19 (2006) 140146

Table 1 23.1 kJ mol
1, respectively. Dutrizac (1986) hypothesized

Correlation coecients for the extraction reactions tted to rst and that activation energies of more than 20 kJ mol
1 are indic-
second order rate equations
ative of a surface reaction control mechanism.
Elements Compounds Correlation coecients In the case of vanadium, the magnitude of the activation
First order reaction Second order reaction energy was 4.96 kJ mol
1 for the rst order reaction, and
Al Al(acac)3 0.9839 0.9297 such a low value is generally considered to be an indication
Cr Cr(acac)3 0.9905 0.9828 of a diusion control mechanism. These statements are
V VO(acac)2 0.8990 0.7517 based on the fact that for chemical, intermediate and diu-
Fe Fe(acac)3 0.9894 0.7060
sion controlled reactions the activation energy (Ea) is usu-
ally >50 kJ mol
1, 2050 kJ mol
1 and <20 kJ mol
1,
indicate a similar maximum percentage recovery as that respectively (Habashi, 1968; Terkel, 1974). It can therefore
obtained at 180 C after 45 min. be expected that physical parameters like agitation, ow of
nitrogen and temperature can inuence the extraction rate
3.4.1. Kinetic analysis of the metals extraction of vanadium signicantly. Conversely for iron the activa-
Table 1 summarizes the rst and second order rate con- tion energy is 181.3 kJ mol
1 which is indicative of large
stants obtained for each of the extraction process, as well potential energy barrier between reactant and product, that
as the respective correlation coecients. It can be seen that must be overcome.
the reactions obey rst order kinetics best.
3.6. Comparison of extraction eciencies
3.5. Activation energies of the extraction processes
The nal results of this investigation are summarised in
The average values for the activation energy for the Table 3. It can be seen from the data in Table 3 that the
recovery of aluminium, chromium, vanadium and iron percentage recovery ranged from 75.2% for iron to 48.2%
with acetylacetone, determined from Arrhenius plots, are for chromium. Despite the large activation energy that
shown in Table 2. must be overcome, iron seems to be very reactive and yields
It can be seen from the data in Table 2 that the activa- the highest recovery in the shortest time at the lowest tem-
tion energies ranged from 4.96 kJ mol
1 to 181.3 kJ mol
1. perature. The fact that Fe(acac)3 had the lowest volatilisa-
The calculated magnitude of activation energy for the tion temperature of all the metal complexes investigated
recovery of aluminium and chromium are 27.7 and could also have contributed to this phenomenon.

Table 2
Optimum conditions for maximum recovery of Al, Cr, V and Fe
Elements Optimum condition for maximum Maximum recovery Activation energy Type of reaction control
recovery (%) (kJ mol
1)
Temperature (C) Time (min)
Al 190 105 63.7 27.7 Surface reaction
Cr 210 150 48.2 23.1 Surface reaction
V 190 120 63.0 4.96 Diusion control
Fe 180 45 75.2 181.3 Chemical reaction

Table 3
A comparison of the percentage recovery of Cr, Al, V and Fe
Methods Conditions Elements Recovery (%) References
Acid extraction 100 C/40 h Cr 5.7 Cohen et al. (1997)
Fe 65.0
Gravity separation Cr 11.5 Khan et al. (2001)
Cr 3.0 Choudhury et al. (1996)
Fe 8.0 Das et al. (1997), Liu (1991)
BFS 1600 C Fe 55.0 Huang and Wang (2001)
Servo process 130235 C Cr 13.6 Allimann et al. (2001)
2 h max V 18.6
Fe 18.7
Gas phase 180 C/105 min Al 63.7 This work
210 C/150 min Cr 48.2
190 C/120 min V 63.0
180 C/45 min Fe 75.2
 J.H. Potgieter et al. / Minerals Engineering 19 (2006) 140146
Table 4
Volatilisation temperature of metal complexes of acetylacetonate
Metals Compounds Mp (C) Volatilisation
temperature (C)
Al Al(acac)3 200 143245
V VO(acac)2 Decompose at 210 131230
Cr Cr(acac)3 215 150230
Fe Fe(acac)3 173 92275
Chromium seems to be the most dicult to recover with
the proposed approach. Numerous recovery methods for
aluminium, chromium, vanadium and iron have been re-
ported. A comparison of the percentage recovery by the
gas phase using acetylacetone to those reported in the liter-
ature by other researchers is given in Table 3.
The dierence in percentage recovery given in Table 3
and those obtained in this investigation may be due to
the dierence in experimental conditions and the type of
feed materials used. However, compared to other metallur-
gical operations and processes, substantially higher recov-
eries can be achieved with the proposed uidised bed
approach than is usually the case. One will have to explore
typical capex and opex costs in more detail to arrive at the
most benecial method of processing and metal recovery in
each case. The current work denitely indicates that the po-
tential of uidised bed technology for waste processing and
metal recovery deserves more attention.
Increasing the temperature of the uidised bed increased
the percentage recovery of the metal up to a certain point,
after which it stayed constant. Allimann et al. (2001) re-
ported similar ndings. These authors found that increas-
ing the temperature from 131 C to 230 C resulted in a
percentage recovery increase of vanadium from y ash up
to 18.60%, iron 18.70% and chromium 13.60%.
Table 4 shows the volatilisation temperature of the metal
complexes of acetylacetone (Allimann et al., 2001; Sievers
and Moisier, 1965). It can be seen that the percentage recov-
ery increases as the volatilisation temperature decreases. An
identical trend was observed by Duke (1985) for the thermal
stability and reactivity of chromium, vanadium and alumin-
ium extracted as coordination compounds.
4. Conclusions
The recovery of valuable metals (Cr, Al, V, Fe) from solid
oxide compounds by gas phase extraction using an organic
extractant, acetylacetone (2,4-pentanedione) was investi-
gated. The focus of the research was to assess the feasibility
of the recovery of metals from solid materials by gas phase
extraction with a chelating agent (2,4-pentanedione acety-
lacetone) at laboratory scale. The nal separation process
of the metal from the complex was not addressed in this re-
search and needs to be investigated further. This investiga-
tion concentrated on the inuence of temperature and
time on the recovery process. The results obtained provide
strong evidence to support the hypothesis that recovering
145
metals from solid compounds by gas phase extraction with
an organic chelating agent is highly feasible. The application
of this technique on industrial scale could provide an indica-
tion of its economic feasibility. In addition the information
obtained relating to the kinetic behaviour of each metal
would be useful in continuous recovery and thus in the de-
sign of this process for practical application. Furthermore,
the process present some advantages such as potential con-
tinuous regeneration of the extractant, easily obtainable re-
agents and easy operation of the reactor.
Acknowledgements
The authors gratefully acknowledge nancial support of
the NRF (National Research Foundation) and the TUT
(Tshwane University of Technology) for this work.
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