Dissolution of Colemanite Process Waste in Oxalic
Acid Solutions
Salih U. Bayca,a Feray Kocan,b and Yuksel Abalib
a
Mining Division, Celal Bayar University, Soma Vocational School, Soma, 45500 Manisa, Turkey; salihbayca@gmail.com (for
correspondence)
b
Chemistry Department, Celal Bayar University, Science and Arts Faculty, 45030 Muradiye, Manisa, Turkey
Published online 12 November 2013 in Wiley Online Library (wileyonlinelibrary.com). DOI 10.1002/ep.11889
The dissolution of colemanite waste in oxalic acid solu-
tions was studied in a batch reactor, and the characteriza-
tion of colemanite waste was determined by X-ray
diffraction analysis and X-ray Fluorescence analysis. The
dissolution parameters in this study were acid concentration,
stirring speed, and reaction temperature, and it was observed
that the dissolution rate increased with increasing reaction
temperature. The experimental data were examined by using
homogeneous and heterogeneous kinetic models, and the dis-
solution kinetics of the waste was determined to be a pseudo-
first-order homogeneous reaction control model. The activa-
tion energy of colemanite waste in oxalic acid solution was
calculated to be 27.80 kJ/mol. Thus, pure boric acid crystals
can be produced using of colemanite waste, and this can
benefit the environment and the economy. V C 2013 American
Institute of Chemical Engineers Environ Prog, 33: 1111–1116,
2014
Keywords: colemanite waste, dissolution, leaching,
kinetics, boric acid, boron oxide, reaction control model
INTRODUCTION
Colemanite is a calcium borate mineral (theoretically,
50.8% B2O3) with a monoclinic crystal structure and a chemical
composition of Ca2B6O11.5H2O or 2CaO.3B2O3.5H2O. In Tur-
key, the boron minerals colemanite, ulexite, and tincal are pro-
duced commercially in large amounts, with colemanite ore
(32% B2O3) produced in open mines in Bigadic, Balikesir
province. The colemanite process is carried out in ore prepara-
tion facilities near the ore mines of Bigadic. Colemanite is
enriched via processes such as crushing, wetting in water,
washing in a tumbler, sieving, triage, and classification, and it
is produced for sale as concentrated colemanite in different
grain sizes and chemical compositions. A major portion of the
concentrated colemanite produced here is exported [1]. The
boron oxide content of the two particle sizes of commercially
produced grounded colemanite is 40 6 0.5 % B2O3 with parti-
cle size of 245 lm and 275 lm [2].
Four fraction particle sizes are produced in the plant. The
products of the concentrator plant are very coarse particle
size of 25–125 mm with 42 6 1% B2O3, coarse particle size
of 3–25 mm with 35 6 2% B2O3, medium particle size of 1–3
mm with 28 6 2% B2O3, and fine particle size of – 1 mm.
The fine particles, which include 17 6 5% B2O3, are pumped
into three waste dams [3].
C 2013 American Institute of Chemical Engineers
V solution, conformity to heterogeneous and homogeneous
Environmental Progress & Sustainable Energy (Vol.33, No.4) DOI 10.1002/ep
Imamutdinova and Zdanovskii reported that when boron
minerals were dissolved in inorganic acid solutions, the reac-
tion products formed a layer on the mineral surface, and this
film resulted in a decreasing reaction rate [4, 5]. Recently, the
dissolution kinetics of colemanite in acid solutions has been
investigated. Alkan et al. studied the leaching kinetics of
colemanite in water saturated with carbon dioxide and
observed that the leaching was controlled by a chemical
reaction [6]. The dissolution of colemanite in aqueous acetic
acid solutions was studied by Ozmetin et al. [7]. They
reported that the dissolution was controlled by a pseudo-
first-order homogeneous reaction. Temur et al. investigated
the dissolution kinetics of colemanite in phosphoric acid sol-
utions and determined that the dissolution kinetics was con-
trolled by a surface chemical reaction [8]. Kucuk et al.
reported that the dissolution of colemanite containing clay
minerals in water saturated with sulfur dioxide was con-
trolled by a chemical reaction model [9]. The dissolution of
colemanite in oxalic acid solutions was investigated by Alkan
and Dogan [10]. They found that the reaction was controlled
by product layer diffusion. Cavus and Kuslu studied the dis-
solution of colemanite in citric acid solutions and observed
that the reaction was controlled by diffusion through the
product layer [11]. The dissolution of colemanite in
(NH4)2SO4 solutions was studied by Tunc et al. [12] who
reported that the dissolution reaction was controlled by a
semiempirical model. Gur et al. studied the dissolution of
colemanite in sulfuric acid solutions at high solid/liquid
ratios and reported that the dissolution reaction was con-
trolled by product layer diffusion [13].
Boric acid is effective in reducing the flammability of cel-
lulose insulation, in cotton batting used in mattresses, and in
wood composites, and is thus used as a fire retardant in
these products [14]. Commercially produced boric acid
(B(OH)3) is 56.25% B2O3, and 99.90% pure. Boric acid is
produced with three different levels of sulfate content. These
are high sulfate with a maximum of 500 ppm SO4, low sul-
fate with a maximum of 130 ppm, and ultra-low sulfate, with
a maximum of 12 ppm [2].
The aim of this study was to investigate the dissolution
kinetics of colemanite waste. This study investigated the dis-
solution of colemanite waste in oxalic acid solutions. Several
experimental parameters were determined for the dissolution
reaction kinetics. The effects of impurities on the reaction
rate were studied. To determine the kinetics and kinetic
model of the dissolution of colemanite waste in oxalic acid
December 2014 1111
Figure 1. X-ray diffraction analysis of colemanite waste. [Color figure can be viewed in the online issue, which is available at
wileyonlinelibrary.com.]

Table 1. Chemical analysis of colemanite waste

Oxides Percent
CaO 29.98
B 2 O3 22.07
SiO2 14.12
MgO 4.87
Al2O3 0.36
Fe2O3 0.43
Na2O 0.02
SrO 0.90
LOI 27.25

mathematical modeling was analyzed by regression analysis.

The activation energy of the dissolution was calculated, and
the parameters, which most affected the speed of dissolution,
were found. This study offers an alternative solution to the
evaluation of the processing of mineral colemanite waste
stored in pools. No study was found in the literature relating
to the dissolution kinetics of colemanite waste. Furthermore,
this study is important in terms of environmental impact Figure 2. The leaching experiment test set-up.
assessment.

MATERIALS AND METHODS

The colemanite ore was processed at Eti Mine Bigadic
Boron Concentrator Plant. The sample (fine fraction) was
taken from the tailing dam. Laboratory tests were performed
on the sample at DEFAM (Experimental Natural Science
Research Center of Celal Bayar University). Chemical analysis
showed that the sample contained 22.07% B2O3. The chemi-
cal analysis results from X-ray fluorescence (XRF) of the cole-
manite process waste (other than B2O3) are given in Table 1.
X-ray diffraction (XRD) analysis of the waste was carried out
on a Rigaku DMAX 2200 Series with Cu Ka radiation. As
seen in Figure 1, the waste was mainly composed of cole-
manite with small amounts of calcite, dolomite, and quartz
minerals.
The test setup was designed to leach the waste and is
shown in Figure 2. The dissolution tests were carried out in
a 500-mL three-neck glass reactor at atmospheric pressure. A
mechanical stirrer with a digital display was used to agitate
the solution. A programmable refrigerated bath/circulator
was used to keep the reaction medium at a constant temper-
ature. A spiral condenser was used to avoid solution loss by
evaporation. The temperature of the solution in the reactor
was measured with a portable digital temperature controller
with a probe and was found to range between 0 and 150 6
0.1 C. Waste was weighed to 0.1 mg using an analytical bal-
ance. A digital chronometer was used to measure the reten-
tion time. The oxalic acid, D-mannitol, sodium hydroxide,
methyl red, and phenolphthalein reagents were of analytical
grade.
During the dissolution process, 100 mL of oxalic acid
solution was placed in the reactor and stirred. After the

1112 December 2014 Environmental Progress & Sustainable Energy (Vol.33, No.4) DOI 10.1002/ep
Table 2. Test variables
Parameters
Reaction temperature ( C) 25 40
Acid concentration (g/L) 40 80
Stirring speed (rpm) 200 500
Reaction time (min) 5 10
Figure 3. Effect of oxalic acid concentration on leaching of
colemanite waste (solid to liquid ratio of 10 g/L, stirring
speed of 200 rpm, at 40 C). [Color figure can be viewed in
the online issue, which is available at wileyonline
library.com.]
Figure 4. Effect of stirring speed on leaching of colemanite
waste (acid concentration of 40 g/L, solid to liquid ratio of
10 g/L, at 40 C). [Color figure can be viewed in the online
issue, which is available at wileyonlinelibrary.com.]
desired reaction temperature was reached, a certain amount
of dried waste was added to the solution. After a certain
period of time, the stirring was stopped. The hot solution
was filtered through filter paper without any change in tem-
perature. The dissolution experiments were repeated at least
twice. The amount of B2O3 in the filtrate was determined by
Environmental Progress & Sustainable Energy (Vol.33, No.4) DOI 10.1002/ep
Values
50 60 70
100
700
20 30 60 120
Figure 5. Effect of reaction temperature on leaching of cole-
manite waste (acid concentration of 40 g/L, solid to liquid
ratio of 10 g/L, stirring speed of 200 rpm). [Color figure can
be viewed in the online issue, which is available at
wileyonlinelibrary.com.]
a volumetric method [15] and the experimental parameters
used in the dissolution processes are given in Table 2. Disso-
lution kinetics calculation method was given by Abali et al.
[16].
RESULTS AND DISCUSSION
Effects of Oxalic Acid Concentration on the Extraction
of the Waste
The experiments were performed in an acid concentration
range of 40–100 g/L acid with a solid/liquid ratio of 10 g/L
and stirring speed of 200 rpm at 40 C, and the results are
given in Figure 3. A great increase in the dissolution rate was
observed with an increase in the acid concentration.
Although the dissolution efficiency rose rapidly in the first 20
min of the experiment, this increase slowed between 30 and
120 min.
Effects of Stirring Speed on the Extraction of the Waste
To determine the effect of stirring speed on the coleman-
ite acid dissolution process, dissolution experiments were
performed with a stirring speed of 200, 500, and 700 rpm at
a temperature of 40 C, a period of 5–120 min, 40 g/L acid
concentration, and a 10 g/L solid-liquid ratio. Results are
given in Figure 4. At 30 min and 200 rpm, a dissolution effi-
ciency of 18.6% was obtained. At 30 min and 500 rpm, this
was 15.3% and at 30 min and 700 rpm it was 15.5%. Maxi-
mum dissolution efficiency was obtained at a stirring rate of
200 rpm. An increase in the stirring rate caused a decrease in
the dissolution efficiency.
December 2014 1113

Figure 6. The variation in 2ln(1 – X) with time at different
acid concentration. [Color figure can be viewed in the online
issue, which is available at wileyonlinelibrary.com.]
Table 3. Variation of dissolution rate with temperatures.
Temperatures (K) k R2
298 0.0149 0.9919
313 0.0387 0.9884
323 0.0403 0.9916
333 0.0626 0.9964
343 0.0662 0.9916
Effects of the Reaction Temperature on the Extraction
of the Waste
To determine the effect of temperature on the acid disso-
lution of colemanite, dissolution experiments were per-
formed at temperatures of 25, 40, 50, 60, and 70 C, a
dissolution period of 5–120 min, a stirring speed of 200 rpm,
a solid-liquid ratio of 10 g/L, and an acid concentration of 40
g/L. Results are given in Figure 5. At 20 min and 25, 40, 50,
60, and 70 C, dissolution efficiencies were 10.34, 16.67,
19.58, 19.58, and 18.62%, respectively. For a dissolution time
of 20 min, dissolution efficiency rose rapidly between tem-
peratures of 25 and 50 C. For a dissolution time of 20 min,
the increase in dissolution efficiency rate slowed between 60
and 70 C. With increasing temperature, the solubility of cole-
manite in oxalic acid solution increased. In this way, the dis-
solution rate of boron oxide at high temperature reached
99.98%.
Kinetic Analysis of Dissolution
The rate of reaction between a solid and a liquid can be
described by heterogeneous or homogeneous-control mod-
els. Fluid-solid heterogeneous reaction systems have impor-
tant applications in chemical and metallurgical processes. A
successful reactor design for this process depends mainly on
kinetic data. Reactions occurring between fluid and spherical
solid particles can be expressed as follows [17]:
Aðf Þ 1 bBðsÞ ! products
Pseudo-first-order reaction-control models were used as
the homogeneous models in this study. The results of the
1114 December 2014 Environmental Progress & Sustainable Energy (Vol.33, No.4) DOI 10.1002/ep
Figure 7. The variation in 2ln(1 – X) with time at different
stirring speed. [Color figure can be viewed in the online
issue, which is available at wileyonlinelibrary.com.]
dissolution rates of waste at different temperatures are given
in Figure 6. These results were analyzed using the equations
of heterogeneous and homogeneous reaction-control mod-
els. The values of these models were plotted against time to
determine their slopes, and the k and regression coefficient
(R2) values of these models for each temperature were calcu-
lated using the slopes of the lines. The leaching kinetics of
waste in oxalic acid solutions did not fit heterogeneous
kinetic models because they did not produce linear relation-
ships. Moreover, the pseudo-second-order homogeneous
reaction-control model did not produce a linear relationship.
However, a high regression coefficient was obtained for the
pseudo-first-order homogeneous reaction-control model. The
kinetics of a pseudo-first-order-reaction-control model is
given by the following equation [17]:
2ln ð12XÞ 5 kt (3)
The first order reaction control models can be fitted due
to linear regression. The regression coefficients and k values
are given in Table 3 for the first order reaction control
model. The results show that the k values increased with the
dissolution temperature.
When the dissolution temperature was increased from 25
to 70 C, the k values increased nearly 4 times. A plot of the
pseudo-first-order homogeneous reaction-control model, –
ln(1–X), versus time results in a linear relationship at differ-
ent acid concentrations as shown in Figure 6, at different stir-
ring speeds as shown in Figure 7, and at different
temperatures as shown in Figure 8.
Okur et al. found that the leaching kinetics of colemanite
in sulfuric acid solutions followed a modified Avrami-type A
model [18]. Sinirkaya et al. obtained a similar result for tincal
waste in CO2-saturated water [19].
Activation Energies
To calculate the activation energy for the dissolution reac-
tion, an Arrhenius graph was drawn using the data in Figure
5. A graph of lnk versus 1/T was drawn using the graph of
the effect of temperature in the acid dissolution of coleman-
ite waste, and Figure 9 was obtained. Table 3 shows the vari-
ation in speed of dissolution of colemanite waste in oxalic
acid solution.

Figure 8. The variation in 2ln(1 – X) with time at different
temperature. [Color figure can be viewed in the online issue,
which is available at wileyonlinelibrary.com.]
Figure 9. Arrhenius plot for the leaching of colemanite
waste. [Color figure can be viewed in the online issue, which
is available at wileyonlinelibrary.com.]
The reaction-control model of colemanite process waste
in oxalic acid solution was determined to follow a pseudo-
first-order homogeneous reaction-control model. The activa-
tion energy of the dissolution was calculated from the Arrhe-
nius Eq. 4 as follows.
k 5 ko exp ð2E=RT Þ (4)
Ln(k) versus 1/T gives a straight line of slope 2E/R. From
the slope of this line, the ko values and the activation energy,
E, of the dissolution rate of waste in oxalic acid were deter-
mined as follows:
2ln ð12XÞ 5 ko exp ð3343:7=T Þ t
E 5 27:80 kJ =mol
Activation energy of 27.80 kJ/mol was calculated from the
slope of the Arrhenius graph of the dissolution of colemanite
waste in oxalic acid solution.
Alkan and Dogan found the activation energy of the dis-
solution of colemanite in oxalic acid solution to be 39.77 kJ/
mol [10]. It has been found that the activation energy of the
Environmental Progress & Sustainable Energy (Vol.33, No.4) DOI 10.1002/ep
reaction controlled by surface chemical reactions is above 40
kJ/mol [20]. The activation energy of colemanite in acidic sol-
utions was reported in the literature to be between 28 and
89 kJ/mol. The activation energy for colemanite dissolution
was studied in phosphoric acid solutions [8]. It was found
that the activation energy of this process was 53.91 kJ/mol.
Kucuk et al. found that the activation energy was 39.53 kJ/
mol for colemanite containing clay minerals in water satu-
rated with sulfur dioxide [9]. Cavus and Kuslu reported that
the activation energy was 28.65 kJ/mol for colemanite in cit-
ric acid solutions [11]. The activation energy was found to be
30 kJ/mol in sulfuric acid solutions [18]. Kum et al. calculated
the activation energy for a solution of calcined colemanite as
89 kJ/mol. Karagolge et al. calculated the activation energy
as 50.6 kJ/mol [21, 22].
In this study, the activation energy of the dissolution of
colemanite waste in oxalic acid solutions was found to be
27.80 kJ/mol. However, the activation energy of the dissolu-
tion of pure colemanite in oxalic acid solutions was found to
be 39.77 kJ/mol [10]. The activation energy of colemanite
waste was lower than the activation energy of pure coleman-
ite. A similar result was also reported by Kucuk et al. [9].
Dissolution Products
The dissolution process of colemanite waste in oxalic acid
solution takes place via the following set of reactions. The
dissolution of oxalic acid is obtained in an aqueous medium
as follows:
C2 H2 O4 :2H2 OðaqÞ ! 2C2 H2 O4ðaqÞ 1 2H2 O (1)
C2 H2 O4ðaqÞ 1 2H2 OðlÞ ! 2C2 O22 1
4 ðaqÞ 1 2H3 O ðaqÞ (2)
The overall reaction is as follows:
2CaO:3B2 O3 :5H2 OðsÞ 1 4H3 O1
ðaqÞ ! 6BðOH Þ3ðaqÞ 1 2Ca
21
1 2H2 OðlÞ
(3)
2CaO:3B2 O3 :5H2 OðsÞ 1 2ðC2 H2 O4 :2H2 OÞðaqÞ ! 6BðOH Þ3ðaqÞ
1 2CaC2 O4ðsÞ 1 2H2 OðlÞ
(4)
The reaction between colemanite and oxalic acid results
in boric acid solution and calcium oxalate solids. Colemanite
waste dissolved in a hot oxalic acid solution and a pregnant
leach solution was formed. Liquid and solid phase were
obtained with filtering the pregnant leach solution. As the
liquid phase cooled, white boric acid crystals were
precipitated.
The output of colemanite mineral processing at a cole-
manite mine is colemanite concentrate and colemanite waste.
Colemanite waste is stored in ponds as a suspension. This
waste is not sold, and constantly requires more storage
space, causing great problems for the environment. In this
study, colemanite waste was turned into a new product,
boric acid, by dissolution in oxalic acid. The sale price of
boric acid is much higher than that of colemanite concen-
trate, and in addition, this study will provide great benefits
to the environment by the reduction in stored wastes.
CONCLUSIONS
The mineral content of colemanite waste was calculated
to be 43% colemanite, while impurities constituted the
remaining 57% of the waste. When the dissolution kinetics of
colemanite waste in oxalic acid solutions was studied in a
batch reactor, the dissolution results showed that the dissolu-
tion rate increased with increasing reaction temperature. The
December 2014 1115
most important parameters in the dissolution rate were found
to be the reaction temperature and reaction time, while the
least important were the acid concentration and stirring
speed. The maximum boron oxide recovery obtained during
dissolution was 99.3% for colemanite waste after 60 min at
70 C. The reaction-control model of colemanite process
waste in oxalic acid solution was determined to follow a
pseudo-first-order homogeneous reaction-control model. Dis-
solution at high temperature was found to be faster than dis-
solution at low temperature. The activation energy of
colemanite waste in oxalic acid solution was calculated to be
27.80 kJ/mol. The activation energy of colemanite waste was
lower than the activation energy of activation energy of pure
colemanite. Pure boric acid crystals were obtained by the
reaction of colemanite waste in oxalic acid. Thus, pure boric
acid crystals can be produced using colemanite waste. This
can contribute to the environment and the economy.
ACKNOWLEDGMENTS
The author would like to thank Eti Mine Works General
Management Turkiye for the XRD, XRF and particle size
analysis.
NOMENCLATURE
k Reaction rate constant (min21)
X Dissolution rate or fractional conversion
t Reaction time (min)
T Temperature (K)
E Activation energy (kJ/mol)
R Universal gas constant (j/mol K)
ko Frequency or pre-exponential factor (min21)
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