Materials Transactions, Vol. 50, No. 5 (2009) pp.

1225 to 1230
#2009 The Japan Institute of Metals EXPRESS REGULAR ARTICLE

Dissolution of Magnesium from Serpentine Mineral in Sulfuric Acid Solution

Kyoungkeun Yoo, Byung-Su Kim, Min-Seuk Kim, Jae-chun Lee* and Jinki Jeong
Minerals & Materials Processing Division, Korea Institute of Geoscience & Mineral Resources (KIGAM), Daejeon 305-350, Korea

As the volume of CO2 , one of greenhouse gases linked to global warming, in the atmosphere increases, there has been an increasing interest
in CO2 sequestration. Aqueous carbonation, which involves the extraction of Mg from serpentine minerals and the subsequent carbonation
reaction with CO2 to form the geologically stable mineral MgCO3 , has been proposed as a promising CO2 sequestration technology. This study
investigates the dissolution of Mg from serpentine mineral in H2 SO4 solution. The study is part of a major research project aimed at developing
an eective CO2 sequestration technology using the serpentine mineral which is readily available in Korea. Complete dissolution of Mg from
natural serpentine was achieved in 30 min at a temperature of 90
C under 0.5 M H2 SO4 . The rate of dissolution of Mg was independent of the
agitation speed at speeds above 300 rpm. The fraction of Mg dissolved from milled serpentine was found to be a little higher than that from
natural serpentine up to 70
C in 0.5 M H2 SO4 . The Jander equation was used to explain the dissolution rate data. The rate of Mg dissolution
seemed to be limited by diusion through the thin channels formed between the silica layers in the serpentine particles.
[doi:10.2320/matertrans.M2009019]

(Received January 16, 2009; Accepted March 11, 2009; Published April 22, 2009)
Keywords: carbon dioxide sequestration, mineral carbonation, serpentine, magnesium, Jander equation

1. Introduction The rate-determining step in the aqueous carbonation of

Serpentine mineral [Mg3 Si2 O5 (OH)4 ] is a hydrous mag-
nesium-rich silicate mineral which generally occurs in three
types: antigorite, chrysotile, and lizardite. It commonly
contains 3238% MgO and 3540% SiO2 with minor
amounts of Fe, Al, Ca, Cr, and Ni.14) Currently, serpentine
has mainly been used as: the ux in blast furnaces in the iron
and steel industry, a road construction material, foundry sand,
fertilizer, and for soil amendment etc.4,5)
Several studies have been carried out to extend the
utilization of serpentine mineral. Pundsack has developed a
method for recovering silica, iron oxide and magnesium
carbonate from serpentine using ammonium bisulfate.6)
Noranda has proposed the Magnola process to produce
magnesium metal from chrysotile serpentine and asbestos
tailing.7) The Magnola magnesium plant with a capacity of
58,000 t/yr was started up in 2000, but was closed in 2003
after operating for about two years. Kosuge et al. have
extensively studied the preparation of magnesium sulfate,
amorphous silica and siliceous porous materials by acid
treatment of the serpentine mineral.8) Kim et al. have
conducted research on the synthesis of zeolite using highly
porous amorphous silica obtained from serpentine by hydro-
chloric acid treatment.9)
As interest increases in the capture and storage of CO2 , one
of greenhouse gases linked to global warming, the avail-
ability of serpentine mineral for sequestering CO2 emissions
generated from fossil fuel combustion has been inves-
tigated.1014) Sequestration of CO2 using serpentine mineral
provides safe, long-term storage for CO2 as CO2 is
immobilized into the mineral by the carbonation reaction to
form thermodynamically stable MgCO3 . Among the carbo-
nation routes for serpentine that have been studied, the most
promising one seems to be the aqueous mineral carbonation
process, which includes the extracting of Mg from serpentine
minerals and the subsequent carbonation reaction with CO2
to form the geologically stable mineral MgCO3 .
*Corresponding author, E-mail: jclee@kigam.re.kr
serpentine minerals is the dissolution of Mg from serpen-
tine.11) Thus, the fundamental characteristics of the dissolu-
tion of Mg from serpentine, which is very important to the
optimization of the mineral CO2 sequestration using serpen-
tine, should be well understood. There have been several
studies on the dissolution mechanisms and kinetics of Mg
from serpentine in acid solutions, but most of them involved
the pre-treatment of the mineral, which aected the dis-
solution of the Mg.1517) Teir et al. have recently reported that
the dissolution kinetics of Mg from natural serpentine in
acids follows a shrinking unreacted-core model with product
layer diusion as the rate-determining step.18) In that study,
the serpentine particles were assumed to be spherical in
shape,18) but serpentine is known to have a layered crystal
structures formed by the alternate stacking of the tetrahedral
silica and octahedral brucite layers.1) Therefore, taking the
crystal structure of serpentine into account,19,20) further
studies are required to completely elucidate the dissolution
of Mg from serpentine in acids.
The present study aimed to examine the behavior of Mg
during H2 SO4 dissolution of the serpentine mineral distribut-
ed in Korea. The eects of H2 SO4 concentration, dissolution
temperature, and agitation speed on the dissolution of Mg
were investigated. The dissolution kinetics of Mg reported in
this paper was determined by minimizing the eects of the
lm boundary diusion and particle size. In addition, the
mechanochemical eect on the dissolution of Mg was
investigated. The study is expected to provide useful data
for the optimization of H2 SO4 dissolution of Mg to
eectively utilize Korean serpentine mineral in CO2 seques-
tration through the aqueous carbonation process.
2. Experimental
2.1 Materials
The serpentine ore distributed in the Andong area, Korea,
was selected for this study. It was ground by a ball mill, and
then sieved to smaller than 45 mm (average particle size
20.6 mm). The X-ray pattern (see Fig. 1) of the serpentine
1226 K. Yoo, B.-S. Kim, M.-S. Kim, J. Lee and J. Jeong

carried out using a 0.5 M H2 SO4 solution by the procedure

A described above.
A : Antigorite C : Chlorite The sample solutions were analyzed by an atomic
D : Diopside F : Forsterite absorption spectrometry (AA, SpectrAA400, Varian Inc.)
M : Magnetite T : Tremolite and an inductively coupled plasma-atomic emission spec-
Intensity (cps)

trometry (ICP-AES, JY-38 plus, Jobin Yvon Ltd.). The

serpentine sample was also characterized by X-Ray Dirac-
tion (XRD) (D-max-2500PC, Rigaku Co.).
A
F 3. Results and Discussion
F
A F
C F F Serpentine is a sheet silicate mineral with a 1 : 1 structure
C C C F A by the alternate stacking of the tetrahedral silica and
T F T F F D
D M octahedral brucite [Mg(OH2 )] layers linked into sheets.
Under acidic conditions, brucite layers of Mg(OH2 ) dissolves
0 10 20 30 40 50 60 70 from serpentine, leaving the silica as a product layer.8,19) The
2 Theta dissolution reaction of Mg from serpentine in H2 SO4 solution
can be expressed as follows:
Fig. 1 XRD pattern of the serpentine ore used in this study.
Mg3 Si2 O5 (OH)4 3H2 SO4
! 3Mg2 3SO4 2 2SiO2 5H2 O 1
Table 1 Chemical composition of serpentine ore used in this study
(mass%).
3.1 Dissolution of natural serpentine ore
Elements Mg Si Fe Al Ca Ni Cr Na K Ig. loss
The dissolution of Mg at agitation speeds in the range 200
Content 19.96 17.52 7.99 2.81 2.62 0.10 0.01 0.07 0.01 8.90 600 rpm was tested to investigate the eect of liquid lm
boundary diusion surrounding solid particles on the rate of
dissolution of Mg from natural serpentine particles in 0.5 M
ore shows that it is composed mainly of antigorite with H2 SO4 at 50
C. As can be seen from Fig. 2, the results
minor lizardite, magnetite (Fe3 O4 ), tremolite [Ca2 Mg5 - indicate that the dissolution rate is independent of the
Si8 O22 (OH)2 ], and diopside (MgCaSi2 O6 ). The chemical agitation speed at speeds higher than 300 rpm. Therefore, in
composition of the serpentine sample which was used all subsequent dissolution experiments, a working agitation
is shown in Table 1. It contained 19.96 mass% Mg, speed of 400 rpm was selected to ensure eective particle
17.52 mass% Si, 7.99 mass% Fe, and 2.81 mass% Al. The suspension in the solution while minimizing the eect of
weight loss of serpentine on ignition for 1 h at 900
C under a liquid lm boundary diusion surrounding the solid particles.
nitrogen atmosphere was 8.90 mass%. The dissolution of Mg from natural serpentine ore was
investigated at H2 SO4 concentrations of 0.13.0 M at 50
C.
2.2 Procedures Figure 3 shows the eect of H2 SO4 concentration on the
Experiments on the dissolution of serpentine in H2 SO4 dissolution of Mg. The fraction of Mg dissolved increased as
solution were carried out in a 1 L three necked Pyrex reactor the concentration of H2 SO4 increased. As shown in Fig. 3,
immersed in a thermostatic water bath. The reactor was tted the rate of dissolution of Mg was initially (in the rst 20
with an agitator and reux condenser. The reux condenser
was inserted in one port to avoid solution losses at high
temperatures. In a typical run, 500 mL of acid solution (0.10 0.8
3.00 M H2 SO4 ) was poured into the reactor and allowed to
Fraction of Mg dissolved, XMg/-

reach thermal equilibrium (2590
C). 2.00 g of serpentine

was then added to the reactor, and the agitator was set to 0.6
400 rpm. During the experiment 4 mL of the solution sample
was taken periodically at a desired time interval (5120 min)
with a syringe. The sample was ltered and then 3 mL of the 0.4
ltrate was diluted with 5% HCl solution for the chemical
analysis. 200 rpm
The milling of serpentine was conducted using a planetary 300 rpm
0.2 400 rpm
ball mill (Pulverisette 5, Fritsch GmbH) to investigate the 600 rpm
mechanochemical eect on the dissolution of Mg in H2 SO4
solution. 25 g of the serpentine sample was placed to a
0.0
jar (250 mL inner volume) with 13 zirconia balls (20 mm 0 20 40 60 80 100 120
diameter). The milling was carried out batch-wise for
Time, t /min
dierent periods of time (30120 min). The rotation speed
of the mill was kept at approximately 150 rpm. Dissolution Fig. 2 Eect of agitation speed on the dissolution of Mg from the natural
experiments with the mechanically activated serpentine were serpentine ore in 0.5 M H2 SO4 at 50
C.
 Dissolution of Magnesium from Serpentine Mineral in Sulfuric Acid Solution 1227

0.8 1.0

Fraction of Mg dissolved, XMg /-

Fraction of Mg dissolved, XMg /-

0.8
0.6

0.6
0.4
0.4 Milling time (min)
H2SO4 conc. (M) 0
0.2 30
0.1 0.25 0.2 60
0.5 1.0
120
2.0 3.0
0.0 0.0
0 20 40 60 80 100 120 0 20 40 60 80 100 120
Time, t /min Time, t /min

Fig. 3 Eect of H2 SO4 concentration on the dissolution of Mg from the Fig. 5 Eect of milling time on the dissolution of Mg from the natural
natural serpentine ore at 50
C. serpentine ore in 0.5 M H2 SO4 at 50
C.

1.0 1.0
Fraction of Mg dissolved, XMg /-

Fraction of Mg dissolved, XMg /-

Temperature (C)
0.8 0.8
25 50
70 90
Temperature (C)
0.6 0.6
25
50
70
0.4 0.4
90

0.2 0.2

0.0 0.0
0 20 40 60 80 100 120 0 20 40 60 80 100 120
Time, t /min Time, t /min

Fig. 4 Eect of dissolution temperature on the dissolution of Mg from the Fig. 6 Eect of dissolution temperature on the dissolution of Mg from the
natural serpentine ore in 0.5 M H2 SO4 . milled serpentine ore in 0.5 M H2 SO4 (Milling time = 30 min).

30 mins) found to be a little fast, but then slowed down
slightly as the dissolution time increased. The fraction of Mg
dissolved increased from about 45% to about 85% as the
H2 SO4 concentration increased from 0.1 M to 3.0 M for a
dissolution time of 120 min.
Figure 4 shows the eect of temperature on the dissolution
of Mg from the serpentine in 0.5 M H2 SO4 solution. The
dissolution temperature varied in the range 2590
C, while
all other parameters were kept constant. It can be seen from
Fig. 4 that higher temperatures yielded higher dissolution
rates of Mg from the serpentine. At 50
C the fraction of
Mg dissolved was about 60% in 120 min, while complete
dissolution of Mg was achieved in 30 min when the
dissolution temperature was increased to 90
C.
3.2 Dissolution of milled serpentine ore
In order to enhance the rate of dissolution of Mg from
natural serpentine ore in H2 SO4 solution, it was mechanically
activated by a planetary ball mill. Figure 5 shows the
dissolution behavior of Mg from the milled serpentine ore in
0.5 M H2 SO4 solution at 50
C as a function of the milling
time. The milling time for the mechanical activation of
natural serpentine ore was varied up to 120 min. As shown in
Fig. 5, appreciable enhancement of Mg dissolution was
achieved through the mechanical activation of natural
serpentine ore by the milling. The speed of the dissolution
of Mg in 0.5 M H2 SO4 solution increased initially (for the
rst 20 min) as the milling time for the natural serpentine ore
increased. Based on the interpretation by Zhang et al.,21) the
somewhat faster dissolution rate of the milled serpentine ore
may explain why the structure of natural serpentine ore was
transformed from a crystalline state into an amorphous one
through the mechanical activation, which was not clearly
veried in this work. Zhang et al. have reported that the
considerable enhancement of the dissolution of Mg from
milled serpentine arises from the structural transformation of
natural serpentine by milling, and that structural transforma-
tion is caused by the disordering around the Mg local
structure caused by the release of the OH base from the Mg
octahedron.21)
Figure 6 shows the eect of the dissolution temperature on
the dissolution of Mg from the milled serpentine ore in 0.5 M
1228 K. Yoo, B.-S. Kim, M.-S. Kim, J. Lee and J. Jeong

0.24
H2SO4 conc. (M)
Experimental data
0.20 0.1 0.25
0.5 1.0
2.0

[ 1 - (1 - XMg)1/3 ]2
3.0
0.16 Best fit line
0.1 0.25
0.5 1.0
0.12 2.0 3.0

0.08

0.04

0.00
0 20 40 60 80 100 120
Time, t /min

Fig. 8 Plot of the results in Fig. 3 according to eq. (2).

in H2 SO4 solution. This was veried after trying a number of

MgO6 octahedral layer
Si2O5 tetrahedral layer
Fig. 7 Schematic model of the structural texture of serpentine ore
(Antigorite type).
H2 SO4 . The serpentine ore was mechanically activated by the
milling at a rotational speed of 150 rpm for 30 min. Figure 6
shows that the dissolution rate of Mg from the milled
serpentine increased remarkably as the dissolution temper-
ature increased. Based on the results shown in Figs. 4 and 6,
it was found that the fraction of Mg dissolved from the milled
serpentine ore was a little higher than that from the natural
serpentine ore in 0.5 M H2 SO4 at a dissolution temperature of
2570
C. However, it was observed that there was little
mechanochemical eect on the dissolution of Mg in H2 SO4
solution when the dissolution temperature was increased to
90
C. This suggests that more information is required about
the feasibility of using mechanical activation to enhance the
rate of dissolution of Mg from serpentine.
3.3 Kinetic analysis
The interpretation of the dissolution kinetics of Mg has
been based on the experimental data for the dissolution of Mg
from serpentine and its textural structure. The textural
structure of serpentine mineral with a 1 : 1 structure due to
the alternate stacking of the tetrahedral silica and octahedral
brucite is shown in Fig. 7.8) In the H2 SO4 dissolution of
serpentine ore, Mg in the brucite layer between the silica
layers dissolves in the acid solution, while the silica which
has not dissolved in the acid solution forms thin channels by
maintaining its own morphology. Thus, it was assumed that
the dissolution of Mg from serpentine ore in the acid solution
proceeds by the diusion of the acid solution throughout the
thin channels formed between the silica layers which may act
as a diusion barrier of H3 O ions. Based on that
observation, the Jander rate equation is expected to best
represent the dissolution reaction of Mg from serpentine ore
dierent rate expressions such as: the spherical shrinking
unreacted-core expression, and the nucleation and growth
equation. The Jander rate equation was derived from the
reactions controlled by a uid diusion mechanism.
This rate expression can be expected to be applicable
because the volume change of serpentine particles before
and after the dissolution of Mg in H2 SO4 solution is
negligible, as can be seen indirectly from the texture of the
serpentine ore in Fig. 7. In this rate expression for a spherical
particle of serpentine ore, the fraction of Mg dissolved
from the serpentine is related to the dissolution time by the
expression:
1  1  XMg 1=3 2 kapp t 2
In this equation, XMg is the fraction of Mg dissolved, t is
the dissolution time (min), and kapp is the apparent rate
constant (min1 ) which is given by
kapp bk f CH2 SO4 bkCH2 SO4 n min1 3
Where b is the stoichiometry factor (b 1=3 in the
serpentineH2 SO4 system, according to the formulation by
Sohn22)) for eq. (1), k is the intrinsic rate constant
(min1 moln ), CH2 SO4 is the concentration of H2 SO4 , f is
the dependence of the concentration of the rate, and n is the
reaction order for the H2 SO4 concentration. It is apparent
from eq. (2) that a plot of 1  1  XMg 1=3 2 vs. t should be
linear with kapp as the slope. The validity of the Jander rate
expression for the dissolution of Mg from the serpentine in
H2 SO4 solution was veried by plotting curves of the
dissolved Mg versus time of Figs. 3, 4 and 6 according to
eq. (2), as shown in Figs. 810. In the present study, the
fraction of Mg dissolved up to 0.90 was investigated for the
kinetic analysis of the dissolution reaction. Figures 810
indicate that the rate of dissolution of Mg is limited by the
diusion of Mg2 , H3 O , and SO4 2 ions throughout the thin
channels formed between silica layers that are not dissolved
by H2 SO4 solution, as explained previously.
In order to evaluate the dependence of the H2 SO4
concentration of kapp , the values of kapp obtained in Fig. 8
was plotted in Fig. 11 as ln kapp against ln CH2 SO4 . As shown
 Dissolution of Magnesium from Serpentine Mineral in Sulfuric Acid Solution 1229

0.28 -6.0

-1
ln (apparent rate constant), k app /min
0.24 -6.5
Temperature (C)
1/3 2

0.20
]

Experimental data
-7.0
25 50
[ 1 - (1 - X Mg)

0.16 70 90
Best fit line -7.5
0.12
25 50
70 90
0.08 -8.0 Reaction order = 0.57

0.04 -8.5
-3.0 -2.0 -1.0 0.0 1.0 2.0
-3
0.00 In (H2SO4 concentration), C H SO /kmol m
2 4
0 20 40 60 80 100 120
Time, t /min Fig. 11 Dependence on H2 SO4 concentration of the dissolution of Mg
apparent rate constants calculated from the results of Fig. 8.
Fig. 9 Plot of the results in Fig. 4 according to eq. (2).

0.30 Temperature (C)

-2.0
Experimental data E For the milled serpentine = 76.7 kJ/mol
0.25 25 50 )
-0.57

70 90
1/3 2

-4.0
ln (k ) (min mol

Best fit line

[1-(1-XMg) ]

0.20
25 50
-1

70 90
0.15
-6.0
0.10
E For the natural serpentine = 82.0 kJ/mol

0.05 -8.0

0.00
0 20 40 60 80 100 120 2.8 3.0 3.2 3.4
Time, t /min 103/T (K)

Fig. 10 Plot of the results in Fig. 6 according to eq. (2). Fig. 12 Arrhenius plot of the rate constants obtained using eq. (4) from the
slopes of each straight line in Figs. 9 and 10.

in Fig. 11, the reaction order n in eq. (3) is obtained to be
0.57 from the slope. Thus, eq. (3) can be rewritten as:
1 T
kapp kCH2 SO4 0:57 min1
3 For the milled serpentineH2 SO4 system
The values of k at dierent temperatures were calculated
using eq. (4) from the slopes of each straight line in Figs. 9
and 10. Figure 12 shows the Arrhenius plots of the rate
constants. The slopes of the straight line placed through
the experimental points yield activation energies of 82.0 kJ/
mol for the natural serpentineH2 SO4 system and 76.7 kJ/
mol for the milled serpentineH2 SO4 system, respectively.
As shown in Fig. 12, the activation energy obtained from
the Mg dissolution experiments of the milled serpentine
ore is a little low compared with that obtained from the
experiments with the natural serpentine ore. Thus, it was
considered that the fraction of Mg dissolved from the
milled serpentine is a little higher than that from the natural
serpentine, as explained previously. The rate constants k
for the natural serpentineH2 SO4 system and the milled
serpentineH2 SO4 system at dierent temperatures calcu-
lated on the basis of eq. (4) can be expressed by the
following equation:
For the natural serpentineH2 SO4 system
 
10 9;862:4
k 7:2  10  exp min1 mol0:57 5
4
 
10 9;225:0
k 1:5  10  exp min1 mol0:57 6
T
Where all the activation energy obtained is a little higher
than measured in many cases of diusion-controlled leach-
ing. In this research, the reason for that was not clearly
determined.19,23) It may be due to some forms of surface
diusion of Mg2 , H3 O , and SO4 2 ions in the thin
channels formed between the silica layers during the
dissolution of Mg, which has a high activation energy. On
the other hand, a number of researchers have also reported a
high activation energy for the diusion-controlled leaching.
Teir et al. have reported that the activation energies for the
diusion-controlled leaching of Mg from natural serpentinite
in several acid solutions are 6874 kJ/mol.18) Hernandez
et al. have also reported that the leaching of Mg from
sepiolite with H2 SO4 has an activation energy of 63.5
kJ/mol,19) which is controlled by diusion of the acid
1230 K. Yoo, B.-S. Kim, M.-S. Kim, J. Lee and J. Jeong
solution. It has also been reported that the activation energies
for the diusion-controlled leaching of iron oxides with HCl
are 6279 kJ/mol.23)
Using eqs. (2) and (4)(6), the fraction of Mg dissolved
from serpentine ore in H2 SO4 solution is, respectively,
represented by the following equation:
For the natural serpentineH2 SO4 system
1  1  XMg 1=3 2 kapp t
Where
 
9;862:4
k 2:4  1010  exp  CH2 SO4 0:57 min1
T 26 (1990) 105118 (in Korean).
For the milled serpentineH2 SO4 system
1  1  XMg 1=3 2 kapp t
Where
 
9;225:0
k 5:0  109  exp  CH2 SO4 0:57 min1
T US Patent No. 3,338,667, (1967).
4. Conclusions
The behavior of Mg during H2 SO4 dissolution of the
serpentine mineral which occurs in Korea was investigated
under diering conditions in a stirred batch reactor. In 0.5 M
H2 SO4 , complete dissolution of Mg from the natural
serpentine was achieved after 30 min at a dissolution
temperature of 90
C. The fraction of Mg dissolved from
the milled serpentine was a little higher than that from the
natural serpentine in 0.5 M H2 SO4 at dissolution temper-
atures up to 70
C, whereas the increase in the fraction of Mg
dissolved was negligible at 90
C. The dissolution kinetics of
Mg were found to follow the Jander equation with the
diusion of Mg2 , H3 O , and SO4 2 ions throughout the thin
channels formed between the silica layers in the serpentine
particles acting as the rate-controlling step. The activation
energies of the dissolution were calculated to be 82.0 kJ/mol
for the natural serpentineH2 SO4 system and 76.7 kJ/mol for
the milled serpentineH2 SO4 system, respectively. The
reaction order with respect to H2 SO4 concentration in the
solution was found to be 0.57.
Acknowledgements
This research was supported by the Basic Research Project
of the Korea Institute of Geosciences and Mineral Resources
(KIGAM) funded by the Ministry of Knowledge and
Economy of Korea. The authors would like to thank Dr.
Young-nam Jang and Dr. Sujeong Lee for providing valuable
comments.
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