RESEARCH FRONT

CSIRO PUBLISHING Full Paper

www.publish.csiro.au/journals/ajc Aust. J. Chem. 2009, 62, 341–347

Processing of Electric Arc Furnace Dust using

Deep Eutectic Solvents

Andrew P. Abbott,A,C John Collins,B Ian Dalrymple,B Robert C. Harris,A

Reena Mistry,A Fulian Qiu,A James Scheirer,A and William R. WiseA
A Chemistry Department, University of Leicester, Leicester, LE1 7RH, UK.
B C-Tech Innovation Ltd, Capenhurst Technology Park, Chester, CE1 6EH, UK.
C Corresponding author. Email: andrew.abbott@le.ac.uk

The present paper describes the design and operation of the first large-scale extraction and separation of metals from a
complex matrix using an ionic liquid. The liquid was a deep eutectic solvent based on choline chloride. The hydrogen-
bond donors were mixed to optimize solubility and fluid viscosity. It was found that the incorporation of a fine particulate
dust actually decreased the viscosity of the fluid. The present paper shows that selective extraction of zinc and lead can
be achieved through judicious choice of the hydrogen-bond donor and it is also shown that metals in solution can be
separated using cementation with zinc powder. Electrowinning of pure zinc is demonstrated but scale-up tests suggest
that the process is relatively slow and has poor current efficiency. An alternative methodology was developed to rapidly
recover the zinc from solution using dilute ammonia solution. It is also shown for the first time that cementation can be
efficiently carried out in ionic liquids because the recovered metal is porous and allows thick layers to be deposited.

Manuscript received: 2 November 2008.

Final version: 7 February 2009.

Introduction
The processing of metal oxides is essential for metal extrac-
tion, waste recycling, and catalyst preparation. One of the
major difficulties with metal oxides is that they are insoluble
in most molecular solvents and generally require strong aque-
ous mineral acids for their dissolution. Separation has usually
been achieved using solvent extraction with specific chelating
agents for given metals. Over the past 10 years, there have been
significant developments in the use of ionic liquids. Ionic liq-
uids have been of considerable interest for a wide variety of
applications including synthesis, electrochemistry, and sepa-
ration science.[1–3] An increasing number of groups are now
using ionic liquids for solvatometallurgical processing. These
are primarily using imidazolium-based liquids and a significant
number of studies have concentrated on uranium processing. Dai
et al.[4] studied the dissolution of UO3 in imidazolium chloro-
aluminate melts. The solubility was found to be in the range
1.5–2.5 × 10−2 M in Lewis basic melts and the main metallic
species in solution was found to be [UO2 Cl4 ]2− . The solvation
of uranium and europium ions in these liquids has been modelled
by Chaumont and Wipff.[5]
Issues associated with water sensitivity of chloroaluminate
melts can be overcome using discrete anions such as PF− 6 and
(F3 CSO2 )2 N− and this is where most studies have focussed
recently. Dai et al.[6,7] have used crown ethers and calixarenes
to extract a range of metals from aqueous solutions. Studies by
Rogers et al. used azonaphthols and crown ethers[8] in a similar
manner.
Recently Visser et al.[9,10] have also developed a new class of
task-specific ionic liquids with monoaza-crown ether fragments
covalently attached to the imidazolium cations and have shown
that they can be used for the biphasic extraction of Cs+ and Sr2+ .
Nockemann et al.[11] have used protonated betaine bistriflamide
salts to dissolve metal oxides such as UO2 , ZnO, CdO, and HgO.
The metal salts can be stripped from the ionic liquids by treatment
with acidic aqueous solutions. The two phases were miscible
above 55◦ C but separated below this temperature.
The area of imidazolium-based ionic liquids with discrete
anions as extraction solvents has recently been reviewed by
Dietz.[12] The review covers the use of neutral and anionic
complexing agents such as crown ethers and organophosphorus
acids. The use of task-specific ionic liquids has been reviewed
separately by Davis.[13]
In a different approach, we have shown that ionic liquids
can also be formed by taking quaternary ammonium salts and
complexing them with simple hydrogen-bond donors (HBD)
such as amides[14] and carboxylic acids.[15] These mixtures form
eutectics where the depression of freezing point can be up to
200◦ C. The mixtures have been shown to have similar solvent
properties to ionic liquids with discrete anions but clearly have
the advantage that they are easier to produce on a large scale,
which has obvious implications for metal recovery processes.[16]
We have shown that these types of ionic liquids can dissolve a
range of metal oxides[17] and they can be used to separate met-
als from a complex mixture using electrochemistry.[18] These
liquids are, however, all totally miscible with water and can-
not be used for biphasic extraction. The solubility of 17 metal
oxides in the elemental mass series Ti through Zn was reported
in three ionic liquids based on choline chloride.[19] This has
also been shown for the practical application of recovering
Zn and Pb from a waste material produced by the electric arc
furnace (EAF).[18]

© CSIRO 2009 10.1071/CH08476 0004-9425/09/040341

RESEARCH FRONT

342 A. P. Abbott et al.

An EAF is one of the most commonly used methods for the 35 Zn

production of steel and is primarily used in the remelting of Pb
scrap steel. The EAF used in steel making and recycling has 30
become a very intensive and rapid process. It involves passing a

Extraction efficiency [%]

high-energy electric current (∼450–500 KWh tonne−1 ) through 25
ferrous scrap and alloying elements to produce molten steel.
Approximately 15–20 kg of dust is formed per tonne of steel 20
but the high content of metals such as Pb and Cd mean that the
waste is classified as toxic. The dust forms when volatile met- 15
als, such as zinc and lead, are vapourized at the high operating
temperature and several million tonnes of dust are produced per 10
annum. There are several different treatment processes that are
either commercial operations or at a developmental stage,[20,21] 5
and these include: high temperature metal recovery, hydromet-
allurgical processes and vitrification or chemical stabilization 0
2 urea 1.5 urea:0.5 EG 1 urea:1 EG 0.5 urea:1.5 EG 2 EG
treatments. In the current work, we demonstrate the optimiza-
tion of the extraction process and the selective cementation HBD composition
of lead.
Fig. 1. Extraction efficiency of Pb and Zn from the arc furnace dust at
50◦ C in deep eutectic solvent of various compositions after 72 h. HBD,
Results and Discussion hydrogen-bond donors.
Small-Scale Optimization
It has previously been shown that using urea-based deep eutec- 3.0  10
7
tic solvents (DES) (1 mol equiv. ChCl:2 urea) offers selective
dissolution of Zn and Pb oxides from EAF dust while showing 2.0  10
7
negligible solubility for iron oxides.[18,19] A process for treating 1.0  10
7
EAF dust will therefore involve three steps: extraction of lead
and zinc from matrix, isolation of lead, and recovery of zinc. The 0.0
I [A]

main issue with the use of the urea-based eutectic is the relatively
high viscosity (∼800 cP at 298 K), which makes it much more
difficult to pump the fluid and to filter the undissolved dust. To
reduce the viscosity of the solvent, different molar amounts of
ethylene glycol were used with urea to form hybrid DESs with
the molar ratio 1:2 (ChCl:HBD).
Fig. 1 shows the extraction efficiency for Pb and Zn from the
arc furnace dust with different molar ratios of DES. These exper-
iments were carried out using 0.1 g of dust and 10 mL of DES. It
can be seen that the extraction efficiency is relatively unaffected
by composition, even down to only 0.5 mol equiv. of urea. The
efficiency for Zn drops significantly, however, with only ethyl
glycol (EG) as the HBD. The viscosity of the 0.5 mol equiv.
of urea liquid was only 56 cP compared with 800 cP in the
1 ChCl:2 urea. For all subsequent studies, the liquid used was the
1 ChCl:1.5 EG:0.5 urea. For all systems, the Fe content was less
than 1 ppm, showing that the extraction efficiency is effectively
zero, ensuring the desired selectivity of the process.
Zinc–Lead Separation
It has previously been shown that electrolysis of EAF dust extract
yields a zinc-rich lead alloy with no traces of any other metals.[18]
What is needed is a selective method to separate zinc from lead in
solution in a quick and efficient way. When the EAF dust was dis-
solved in the hybrid solvent, the resulting voltammogram showed
a significant difference from that in 1 ChCl:2 urea previously
reported.[18] Differences have also been observed for the depo-
sition of Zn–Sn alloys in urea- and ethylene glycol-based liquids
and these have been ascribed to differences in speciation.[22]
Fig. 2 shows that separate signals for the two metals are observed
and these are separated by ∼500 mV, which suggests that the
metals could be separated potentiometrically; however, practi-
cally this is difficult to scale up and leads to impure products. A
common alternative in aqueous solutions is cementation. In this

1.0  10
7

2.0  10
7 Pb

3.0  10
7
Zn

4.0  10
7

1.0
0.8
0.6
0.4
0.2 0.0 0.2 0.4 0.6
E [V]
Fig. 2. Cyclic voltammogram at 0.5-mm Pt disc electrode in
ChCl/urea/ethylene glycol (1:0.5:1.5) after extraction of electric arc furnace
dust (scan rate = 20 mV s−1 ).
process, a sacrificial metal with a more negative redox poten-
tial than the metal being recovered is immersed in the solution.
The metal ions in the liquid are reduced and deposited onto the
sacrificial metal, which in turn is oxidized and goes into solu-
tion. In aqueous solutions, this tends to be an inefficient process
because the immersion deposit is dense and precludes dissolu-
tion of the underlying metal. Although cementation to recover
metals from solution has not been used before for ionic liquids,
we have recently shown that immersion deposits of silver on cop-
per and copper on aluminium can be obtained.[23] The deposits
are porous and sustained deposition can be achieved. For the
current case, the process is Pb2+ + Zn(s)
Pb(s) + Zn2+ , which
is ideal because zinc metal is an inexpensive substrate that will
be recovered in the final stage of the process.
A sample of EAF dust was extracted using the 1 ChCl:1.5
EG:0.5 urea mixture at 50◦ C for 2 days. The resultant liquid was
filtered and a zinc sheet was immersed for 2 days at 25◦ C. At
the end of this time, a black deposit was produced and energy
dispersive X-ray spectroscopy (EDAX) analysis of the sample
showed the only metal present on the surface was lead. This
 RESEARCH FRONT

Processing of Electric Arc Furnace Dust 343

100

2h
8.0  10
6 4
80
6
8
6.0  10
6

% Pb extracted
20
0 60
I [A]

4.0  10
6
40

2.0  10
6
20
0.0

1.0
0.5 0.0 0.5 1.0 0

0 2 4 6 8
E [V] Time [h]

Fig. 3. Anodic stripping voltammetry for 3.4 × 10−3 mol dm−3 PbCl2 in 1 ChCl:0.5 urea:1.5 EG at 50◦ C (scan rate = 20 mV s−1 ). A Zn sheet, area: 14 cm2 ,
was immersed in the liquid and voltammograms were run after different lengths of time (left) and graph of lead extracted as a function of time (right).

60 1.16
Neat
Neat
1 wt-%
50 1.14 1 wt-%
2 wt-%
5 wt-% 2 wt-%
1.12 5 wt-%
40 10 wt-%
10 wt-%
Density [g cm
3 ]
Viscosity [cP]

1.10
30
1.08
20
1.06
10
1.04

0 1.02
20 30 40 50 60 70 80 20 30 40 50 60 70 80
Temperature [C] Temperature [C]

Fig. 4. Viscosity (left) and density (right) as a function of temperature for a 1 ChCl:1.5 EG:0.5 urea deep eutectic solvent containing various amounts of
electric arc furnace dust.

shows that cementation can be used as a method for achieving
effective separation of Pb from Zn in the EAF dust.
To determine the kinetics of lead cementation, voltammetry
for 3.4 × 10−3 mol dm−3 PbCl2 in 1 ChCl:0.5 urea:1.5 ethy-
lene glycol at 50◦ C was performed (note: no ZnCl2 present).
A Zn sheet (area = 14 cm2 ) was immersed in 10 mL of the liq-
uid and voltammograms were run after different lengths of time.
The results are shown in Fig. 3. This looks different from the
anodic response in Fig. 2 as no alloy is being formed. From
the area under the peaks, the concentration of lead remaining in
the liquid was determined and the rate of extraction was found
to be 3 × 10−7 mol cm−2 h−1 . The experiment in Fig. 3 was
repeated with a considerably decreased amount of Zn powder
(0.02 g = 1.5 equiv. of Zn) added to 3.4 × 10−3 M PbCl2 dis-
solved in a mixture of 1 ChCl:0.5 urea:1.5 EG. The high surface
area of zinc dust means that almost all the lead can be extracted
in the above solution in ∼10 min, using significantly less Zn
than in the sheet. This shows that cementation is an extremely
effective method of extracting lead from the solution.
Electrolysis of the resulting liquid using a mild steel cathode
at a current density of 2.5 A dm−2 resulted in the deposition of
a thick, dark grey metallic film. EDAX confirmed that this was
only zinc with no traces of lead. Based on the above protocol,
a series of scale-up experiments were performed using 75 kg of
liquid and 5 kg of dust.
Scale-Up
Dust Loading
The first issue to be addressed was one of dust loading in the
DES for the large-scale experiments. In aqueous solutions, the
addition of finely divided dust causes a significant increase in
the solution viscosity. The effect of EAF dust loading on vis-
cosity and density of the ChCl:urea:EG hybrid was determined
as a function of dust loading weight and temperature. Fig. 4
shows that when 1 wt-% EAF dust is added to the ionic liquid,
the viscosity decreases by ∼50% at all temperatures. This is a
remarkable observation and has also been observed for other
small particle species in these DESs.[24]
Ionic liquids in general are viscous and it has been shown
that this is due to the large ions and the small void volume in the
liquid.[25] The decrease in viscosity on addition of solid can be
explained by the dust particles breaking up the structure of the
ionic liquid. Movement of the particles will cause microscopic
stirring and allow improved mass transport. This is potentially a
very useful concept for improving mass flow in ionic liquids. The
RESEARCH FRONT

344 A. P. Abbott et al.

Zn dust

EAF dust
Electrolysis cell

Zn

Zn/Pb/Cd
Pb

Cementation tank

Leach tank

Fig. 5. Schematic diagram of the cell for extracting lead and zinc from electric arc furnace (EAF) dust together with a photograph of the pilot plant built
for 5 kg dust extraction batches.

addition of up to 5 wt-% causes no further change in viscosity. 80

The addition of 10 wt-% causes an increase in the viscosity but it
is still lower than that of the pure fluid. The addition of dust also 70
has a negligible effect on the density of the liquid, presumably 60
because the dust has a similar density to the ionic liquid, which
Extraction efficiency

can be seen in Fig. 4.The effect of the particulates on the structure 50

is difficult to quantify because the solubility of metals will have
Zn
an effect on viscosity. However, recent analogous studies with 40
Pb
alumina, which is insoluble, showed that the effect is real and it
was possible to show that there is an increase in free volume of 30
∼17% when 0.05-µm particles are added.[24] It was decided for
20
the large-scale experiments to use a dust loading of 7 wt-%.
Fig. 5 shows schematically the pilot plant that was built for 10
the extraction process. The main extraction tank has a capacity
of 125 L and there were 2 × 25 L tanks in which batches could be 0
treated to remove lead using cementation with Zn dust, followed 0 500 1000 1500 2000 2500 3000
by a 12-L electrolysis cell. Fig. 5 also shows a photograph of the t [min]
plant constructed for this purpose.
Fig. 6. Extraction efficiency of Pb and Zn from the arc furnace dust at
50◦ C in the hybrid deep eutectic solvent as a function of time.
Extraction Efficiency
Fig. 6 shows the extraction efficiency for the same batch of EAF that the zinc was present in several forms including franklin-
dust at a 5-kg scale as a function of time. Comparison of Figs 1 ite, ulvospinel, and small quantities of cuprospinel. Franklinite
and 6 shows that scale-up improves the extraction efficiency for was by far the major spinel structure found. It can exist in sev-
zinc although the extraction of lead is slightly decreased. This eral different forms, the main one of which has the formula
may be because the solution is close to its saturation concen- (Zn,Mn,Fe)2+ (Fe,Mn)3+ 2 O4 , and the spinel has an isometric
tration for total metal content. The increased extraction of zinc crystal system. Ulvospinel has the formula Fe2TiO4 and also
compared with the small scale is probably due to increased stir- has an isometric crystal system. These materials are notoriously
ring, which allows better mixing of the dust and DES. Although difficult to dissolve in aqueous media; however, as they typically
increased solubility was obtained, not all of the zinc could be constitute half of the dust, the DES is probably dissolving some
extracted even after 72 h. This could be due in part to the speci- of these phases in the large-scale experiment, albeit slowly.[26,27]
ation of the zinc. X-Ray powder diffraction analysis was carried It can be seen from Fig. 6 that a significant amount of the Zn
out on the undissolved dust after extraction and it was found has dissolved after 24 h, which is a viable time for an extraction

Processing of Electric Arc Furnace Dust
35000
30000
Concentration [ppm]
25000
20000
15000
10000
5000
0
0 20 40 60 80 100
Time [h]
Fig. 7. Concentration of zinc as a function of time during the depletion test
carried out at 3.5 A.
time. Clearly, by increasing the temperature, extraction rates, and
possibly efficiency can be improved, but this is a parameter that
still has to be optimized. Filtration on a small sale was carried
out using a 0.45-µm mesh filter and syringe. This resulted in a
clear solution. On a large scale, the DES was filtered through
a double bag filter (both 1-µm mesh size) and this removed
the majority of the suspended particulate matter (which was
in the range 0.5–3 µm). There was still a significant turbidity
to the solution and the filtration is still an issue that needs to be
addressed, although it is not significantly different to filtration
of any other fine particulate suspension.
Pb Cementation
A 20-L aliquot was taken from the extraction tank and 100 g of
zinc dust was added. After 2 h, a sample of DES was taken and
the Zn and Pb concentrations were determined using inductively
coupled plasma–atomic emission spectrometry (ICP-AES).
The Pb concentration was reduced by 75% and a concomitant
increase in the Zn concentration was observed, showing quan-
titative exchange of the two metals in solution. The experiment
was repeated four times and the residual lead concentration was
found to be 12 ppm on average, which was close to the back-
ground level. The amount of lead removed depended strongly
on the concentration of zinc in solution. When the zinc concen-
tration was 4000 ppm, 97% of the lead was removed but when the
Zn concentration was 12000 ppm, only 63% was removed. This
would be expected because the difference between the Zn2+/0
and Pb2+/0 couples will be governed by the Nernst equation,
which will accordingly affect the equilibrium constant. Inter-
estingly, on cementation, the lead aggregated to form large
‘shot’-sized clusters that settled rapidly to the base of the cell,
simplifying separation.
Zn Recovery
Following the cementation step, a 10-L aliquot was run into the
electrolysis tank. This was fitted with a steel cathode (surface
area = 456 cm2 ) sandwiched between two iridium oxide-coated
titanium plate anodes, each of similar surface area. The solutions
were electrolyzed at constant voltage and samples were taken at
regular intervals to determine the residual Zn levels in solution.
Fig. 7 shows the concentration of zinc in solution as a func-
tion of time and applied voltage. The cathode was also weighed
RESEARCH FRONT
345
2A
2.5
80
3
3.5
70 4
5
Current efficiency [%]
6
60
50
40
30
120 20
2 3 4 5 6 7
Time [h]
Fig. 8. Current efficiency for the electrowinning of zinc from the hybrid
deep eutectic solvent at 50◦ C as a function of applied current.
to determine the current efficiency of the process. These data
are shown in Fig. 8. It can be seen as in most electrowinning
processes that the current efficiency decreases as the applied
voltage increases such that the efficiency is relatively poor (75
to 32%) with voltages that yield reasonable deposition rates. The
extraction efficiency also decreases as the zinc concentration in
solution decreases. Exhaustive electrolysis was carried out over
a 72-h period, at the end of which the cathodes were analyzed
using EDAX. It was found that there were no traces of lead in
the deposit. The zinc morphology is shown through an scanning
electron microscopy image of the surface in Fig. 9, together with
a photograph of the electrode.
The results in Figs 7 and 8 show that the electrowinning of
zinc from solution is slow and current-inefficient and probably
economically unfavourable on a large-scale owing to the low
value of zinc metal. An alternative approach would be to pre-
cipitate the metal from solution with a complexing agent that
forms an insoluble species. This has the potential advantage that
a higher-value product could be obtained.
It has previously been shown that iron, chromium, and nickel
could be precipitated from a DES that had been used for elec-
tropolishing by the addition of an equal volume of water.[28] The
DES was filtered and regenerated by evaporating off the water.
This was attempted with the leachate from tank 2 but found to be
ineffective at precipitating zinc. It is well known that ammonia
solution is an extremely effective precipitating agent for zinc in
aqueous solutions.[29] Various concentrations of ammonia solu-
tion were added to aliquots of the leachate and the results in
Fig. 10 show that dilute solutions are extremely effective at pre-
cipitating Zn from solution. This is most likely due to partial
ammination of Zn that is not as soluble in the ionic liquid/water
as the fully amminated Zn species.[29] The rate of precipitation
was greatest in the 1.75 mol-% and 3.5 mol-% solutions, with
an almost immediate precipitation being observed. In the higher
concentrations, the precipitation took longer and in the 26 and
35% tests, the precipitation occurred after being left overnight at
3◦ C. Small-scale tests showed that this liquid could be regener-
ated by filtration and then evaporation of the ammonia solution
from the liquid. The resulting liquid was slightly depleted of urea
owing to decomposition at higher temperatures but this could be
easily added to bring the liquid back to its original composition.
RESEARCH FRONT

346 A. P. Abbott et al.

Acc.V Spot Det WD 20 µm

20.0 kV 5.0 SE 9.7

Fig. 9. Scanning electron microscopy (left) and photograph (right) of cathode after 7 h electrowinning at 50◦ C, 2.5 A, and at 40 rpm pump speed.

30000 Table 1. Average composition of electric arc furnace dust

25000 Element analyzed Average wt-% composition

Zn 33.2
20000 Pb 2.7
Zn [ppm]

Fe 33.3
Mn 3.7
15000 Ca 5.7
Mg 1.8
10000

5000

5 0 5 10 15 20 25 30 35
Ammonia concentration in solution [%]
Fig. 10. Plot of Zn concentration remaining in ionic liquid after washes
with various concentrations of ammonia solution.
Conclusions
The present work shows that metals can be extracted from solid
matrices using DESs. Effective separation can be achieved by
selective dissolution through appropriate choice of the HBD,
cementation of the metal in solution, electrowinning of the
metal in solution or precipitation of the metal by addition of an
aqueous-based complexing agent. This is a generic technology
that could be applied to a wide variety of matrices. The simplic-
ity in terms of synthesis and constituents means that this can be
applied to large-scale extraction. The inclusion of powders does
not unduly affect the liquid viscosity as the particles increase
the free volume of the liquid and actually aid mass transport.
The process for extraction of lead and zinc from EAF dust was
optimized using 1 ChCl:0.5 urea:1.5 EG mole equivalents to
maximize solubility while minimizing viscosity. A dust loading
of 7 wt-% was used, although solubility experiments suggest that
this could be raised before the zinc concentration becomes sat-
urated. The minimum digestion time was 24 h but cementation
of the lead from solution could be achieved using finely divided
zinc dust in ∼10 min. Zinc chloride could be precipitated from
the solution by the addition of 2 mol-% ammonia solution.
Experimental
40
Choline chloride [HOC2 H4 N(CH3 )+ −
3 Cl ] (Aldrich, 99%) was
recrystallized from absolute ethanol, filtered, and dried under
vacuum. Urea and ethylene glycol (both Aldrich, >99%) were
used as received. The mixtures were formed by stirring the com-
ponents together at 100◦ C until a homogeneous, colourless liquid
formed. The viscosity was determined using a Brookfield DV-E
viscometer fitted with a thermostatted jacket. Metal solubility
was determined by placing 0.1 g of the metal oxide (various
sources, all >98%) in 10 mL of the ionic liquid for 3 days at
50◦ C. The solution was filtered at 50◦ C, diluted with 0.1 M HCl
and analyzed using a JY Ultima 2 ICP-AES. The EAF dust is
highly variable in composition depending on the batches of scrap
used. For the current research, one sample was used and the aver-
age content of metals is shown in Table 1. The pilot plant was
custom-built by C-Tech Innovation Ltd (Chester, UK).
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