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Utilization of formic acid solutions in leaching reaction kinetics of natural

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DOI: 10.1016/j.hydromet.2014.08.008

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Hydrometallurgy 149 (2014) 183–188

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journal homepage: www.elsevier.com/locate/hydromet

Utilization of formic acid solutions in leaching reaction kinetics of natural

magnesite ores
Nadeem Raza ⁎, Zafar Iqbal Zafar, Muhammad Najam-ul-Haq
Institute of Chemical Sciences, Bahauddin Zakariya University, Multan, 60800, Pakistan

a r t i c l e i n f o a b s t r a c t

Article history: In the present research work, dissolution kinetics of natural magnesite is carried out using formic acid as a
Received 12 November 2013 leaching agent. The effect of various reaction parameters such as temperature, acidic solution concentration, par-
Received in revised form 22 June 2014 ticle size and liquid to solid ratio was studied regarding the leaching kinetics of natural magnesite. The findings
Accepted 16 August 2014
show that the dissolution process is controlled by the chemical reaction (intrinsic) at the liquid-solid interface;
Available online 24 August 2014
1=3 1 −42078=RT
Keywords: 1−ð1−xÞ ¼59:41  10 e t:
Magnesite
Formic acid The apparent activation energy of the leaching process of magnesite with the formic acid was found to be
Dissolution kinetics 42.08 kJ mol−1 over the reaction temperature range of 318 to 348 K.
Regression analysis © 2014 Elsevier B.V. All rights reserved.
Kinetic model

1. Introduction
Magnesium, the 6th most common element, does not occur freely in
nature because of its high reactivity. It is abundant in magnesite, peri-
clase, asbestos, meerschaum, serpentine, talc and epsomite (Deangelis
et al., 2007). Magnesium is important in many aspects of life and its
uses involve synthesis of Grignard reagent, alloy formation, sulfur
removal in iron and steel production, refractory materials, fertilizers,
medicinal products, and fireproofing (Bukovisky, 1997; Jones et al.,
2000).
A wide range of studies have been reported on leaching and dissolu-
tion kinetics of rocks with a variety of leaching agents (Demirkiran,
2008, 2009; Demirkýran and Künkül, 2007; Demirkiran and Kunkul,
2008; Dogan and Yartasi, 2009; Kovacheva et al., 2001; Kuslu and Colak,
2010; Mergene and Demirhan, 2009; Sandstrom and Samuelsson, 2010;
Zhang and Nichol, 2010). In these research studies, it has been described
that the leaching kinetics of different metal ores may vary with the
change in nature and type of rock deposits. Leaching of magnesite
rocks can be achieved by acids (inorganic/organic) or bases and their
salts (Lacin et al., 2005). The studies on the dissolution process of mag-
nesite in inorganic acids such as HCl, H2SO4 (Abali et al., 2006; Chou
et al., 1989) showed that the controlling mechanism for the
dissolution of magnesite is a chemical process. Inorganic acids have
issues of selectivity, froth formation and scaling (Housmanns et al.,
⁎ Corresponding author. Tel.: +92 300 6340861.
E-mail address: nadeemr8@hotmail.com (N. Raza).
1996). Conversely, organic acids can act as active leaching reagents be-
cause most of the leaching reactions are done in mild acidic conditions
(pH 3–5). Moreover, organic acids have a low risk of corrosion and
can be utilized for carbonaceous rocks. Another advantage of organic
acids as leaching agents is their biodegradability, which generally de-
pends on the carbon chain and other attached groups.
From leaching investigations of naturally occurring magnesite mate-
rials in acetic acid, gluconic acid, citric acid and lactic acid solutions, it
was found that leaching kinetics were driven by chemically controlled
mechanisms (Bayrak et al., 2010; Lacin and Bakan, 2006; Lacin et al.,
2005).
Magnesite ore deposits are found abundantly in the Khuzdar areas of
Balochistan (Pakistan). The Khuzdar area consists of a number of
Kraubath type magnesite deposits associated with alpine type bela
ophiolite dating from the cretaceous period (Bashir et al., 2009). These
are mostly serpentinized and harzburgite confined mostly in the
lowermost segment of bela ophiolite. These deposits have not been
considered extensively for leaching kinetic investigations up to this
time. Moreover, no literature has been reported concerning formic
acid as a leaching agent for the study of leaching kinetics of indigenous
magnesite.
Therefore, the current research work was intended to investigate the
leaching reaction kinetics of the indigenous magnesite ore by formic
acid. The product formed (magnesium formate) can be used in animal
feed formulations and in general chemical applications (Shi et al.,
2005). It can also be used for determining pesticides in fruits and vege-
tables and for the simultaneous determination of tropane alkaloids and
glycol alkaloids in grains and seeds.

http://dx.doi.org/10.1016/j.hydromet.2014.08.008
0304-386X/© 2014 Elsevier B.V. All rights reserved.
 Author's Personal Copy
184 N. Raza et al. / Hydrometallurgy 149 (2014) 183–188
2. Experimental procedures
2.1. Sample protocol and analyses
Samples of magnesite involved in the current study were collected
from the Khuzdar area in the province of Balochistan (Pakistan).
Samples were ground in a ball mill followed by a mortar grinder. Differ-
ent size fractions (500–707, 250–354, 177–210 and 125–177 μm) were
obtained from screening of ground samples by ASTM sieves, and then
dried in an electric oven at 100 °C for 24 h. These samples were brought
to room temperature and stored. Atomic absorption spectrometry,
scanning electron microscopy and other conventional methods
(Furmann, 1963) were applied for the analysis of magnesite rock frac-
tions. The formic acid (methanoic acid), EDTA (ethylene diamine tetra
acetic acid) and EBT (eriochrome black T) used during analysis were
of reagent grade. The preparation of stock solutions and their further
dilutions were made using deionized water. Eriochrome black T and
EDTA were used in volumetric quantitative determinations of magne-
sium in leached solutions. In complexometric titrations of magnesium
(Gulensoy, 1974), EBT acts as an indicator while EDTA is used as a
complexing agent for Mg.
2.2. Detection measurements and analytical procedure
Atomic absorption spectrophotometer (Hitachi-1800) was used for
the determination of Mg in natural magnesite samples. Scanning elec-
tron microscope (JEOL JED-2300) was used to observe the particle mor-
phology of raw magnesite. Leaching studies of magnesite samples were
investigated in a reactor made up of glass with 500 mL capacity. A hot
plate (IKA C-MAGHS-7) equipped with a temperature sensor (ETS-D5)
was used to stir, heat and control the temperature (± 0.5 K) of the
reactor contents. In each experiment, a fixed volume of 8% formic acid
having an L/S ratio of 14:1 mL/g was gradually introduced to the reactor
with 5 g of sample. These entities were agitated with stirring rate of
350 rpm at known times and temperatures. After completion of the
reaction, the hot solution was filtered to remove gangue minerals
from magnesium formate. The filtrate solution was analyzed to find
the percentage of conversion of magnesite (Gulensoy, 1974).
3. Results and discussion
3.1. Sample characterization
To find loss on ignition, magnesite rock samples were heated to
950 °C for 24 h in a furnace. The carbonates of different elements
were converted into their oxides with the liberation of CO2. The chemi-
cal composition of the calcined magnesite sample (Table 1) was deter-
mined by atomic absorption spectrometer. Table 1 indicates that
magnesium is present in relatively higher concentrations than the
other elements. The EDX spectrum of the intact ore of magnesite
(Fig. 1) depicts the elemental composition. The elemental composition
showing the mass and atomic % of different elements in the indigenous
magnesite is given in Table 2. From the EDX signature, it can be inferred
Table 1
Chemical composition of natural magnesite orea.
Component (Mass.%)
MgO 43.47
CaO 0.38
Fe2O3 1.11
SiO2 1.54
Loss on ignition (at 950 °C for 24 h) 53.5
a
Results obtained from analysis of magnesite ore by AAS (Hitachi-1800).
that the material under study is magnesium rich. The profile also
exhibits the presence of carbon and oxygen indicating the presence of
carbonates. The magnesite in pure form is usually white in appearance
but becomes colored due to the inclusion of impurities. The SEM
image of the raw magnesite ore representing the apparent morpholog-
ical properties of the magnesite is given in Fig. 2. The material appears to
be non-granular with surface roughness, which may be due to the
evolution of volatiles during the weathering and formulation of the ore.
3.2. Chemical reactions taking place in the glass reactor
Chemical reactions occurring in the reaction vessel containing
magnesite and formic acid solution is represented as:(a) Formic acid
ionization
þ ‐1
CH2 O2 ↔H þ CHO2 ð1Þ
(b) Diffusion of H+ ions(c) Attack of H+ ions on the magnesite particles
þ 2þ
2H þ MgCO3 ↔H2 CO3 þ Mg ð2Þ
(d) Reaction between Mg2+ and formate ions
2þ −1
Mg þ 2CHO2 ↔MgðCHO2 Þ2 ð3Þ
The ionization constant of formic acid is pKa = 3.75 at 20 °C and the
solubility product constant for MgCO3 is 6.8 × 10−6 at 25 °C (Harned
and Embree, 1934; Visscher et al., 2012). Ashraf et al. (2005) described
that the magnitudes of the constants (ionization constant and solubility
product constant) are generally temperature dependent and efficiency
of the leaching reaction is restricted by the kinetics.
3.3. Effect of time and reaction temperature
The reaction temperature was varied from 45 °C to 75 °C to eluci-
date the influence of temperature on the rate of dissolution of magne-
site while keeping the other experimental conditions constant (177–
210 μm particle size, 8% formic acid, liquid/solid ratio of 14:1 mL/g
and stirring speed of 350 rpm). The results are shown in Fig. 3, which il-
lustrates that an increase in reaction temperature causes a rise in the
rate of conversion of the magnesite. The elevation of reaction tempera-
ture from 55 °C to 75 °C in 30 min causes an increase in % recovery of
magnesite from 49.8% to 84.9%. This situation indicates that an increase
in the reaction temperature increases the rate of chemical reaction. Typ-
ical rate curves in Fig. 3 represent the temperature increase, which re-
duces the reaction time needed to achieve the maximum conversion.
About 95% dissolution of magnesite is achieved at 75 °C in 40 min of
leaching time. A number of experiments were carried out to determine
the effect of formic acid concentration, L/S ratio in the medium and the
particle size of magnesite on the dissolution kinetics of magnesite at
65 °C.
3.4. Influence of acid concentration and L/S ratio
In order to find the influence of concentration of formic acid on the
leaching of magnesite, the concentration of formic acid was varied
from 2% to 10% at a temperature of 65 °C, stirring rate 350 rpm and par-
ticle size fraction 177–210 μm. The results are shown in Fig. 4, which
shows that an increase in acid concentration accelerates the rate of
leaching of magnesite. However, concentrations higher than 8% do not
have an appreciable effect as expressed in Fig. 4. This situation may be
attributed to the fact that a relatively higher concentration of the
leaching agent may attack the gangue minerals present in the ore.
Ozmetin et al. (1996) described that an increase in the concentration
of leaching agent in the reaction vessel may increase the product layer
formation and produce a solid film layer surrounding the particles and
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N. Raza et al. / Hydrometallurgy 149 (2014) 183–188 185

Fig. 1. The EDX pattern of natural magnesite.

this may reduce the rate of the leaching process. The influence of the liq- 4. Kinetic analysis
uid/solid ratio was elucidated by varying the L/S ratio from 6:1 to
16:1 mL/g, keeping the other experimental parameters constant. Exper- Hydrometallurgical processes usually involve solid–liquid reaction
imental results have been expressed in Fig. 5. The rate curves in Fig. 5 systems. In solid–liquid reactions, the leaching kinetics is governed
show that an increase in the L/S ratio causes an improvement in the dis- (Lacin et al., 2005; Levenspiel, 1972) by one of the following mechanisms:
solution of magnesite. However, its effect on the leaching process is not
a) Diffusion from fluid films
as dominant as that of the temperature and formic acid concentration.
b) Ash to product layer
Higher liquid/solid ratio results in an increase of volume of leaching
c) Chemically controlled reactions
agent and a modification of the ratio between Mg and formic ions.
Moreover, the increased volume of the reaction mixture may increase The outcome was examined from the shrinking core model to eval-
filtration time and its handling process. uate the rate-determining step and reaction conditions affecting
leaching kinetics of magnesite. On these grounds, a general reaction of
solid with fluid can be expressed as:
3.5. Influence of particle size of magnesite
AðfluidÞ þ bBðSolidÞ →product ð4Þ
Various experiments were performed to probe the particle size im-
pact. The leaching kinetics of magnesite were performed using 4 sample
sizes (500–707, 250–354, 177–210 and 125–177 μm) at 65 °C, 8% Only two controlling mechanisms (diffusion from fluid films or
formic acid solution, stirring speed of 350 rpm and a liquid/solid propor- chemically controlled reaction) may be considered during the reaction
tion of 14:1 mL/g. The results are summarized in Fig. 6, which shows if no ash/product layer is produced. If the conversion fraction of natural
that the increase in particle size of magnesite samples has an inverse magnesite is x at any interval t, then the integral rate equations for
impact on the dissolution process. This situation may be related to the fluid–solid systems can be denoted as:
fact that with the decrease in particle size of the magnesite, the surface For the film diffusion controlling mechanism,
area of the particles for reaction may become more available for the
leaching process.
t ¼ ko ½1−ð1−xÞ  ð5Þ

Table 2
Elemental analysis of natural magnesite orea.

Element (keV) (Mass %) (Atomic %)

C 0.277 14.591 20.446

O 0.525 57.567 60.501
Mg 1.253 26.086 18.2767
Si 1.739 0.7186 0.4314
Ca 3.690 0.268 0.1127
Fe 6.398 0.7728 0.2321
a Fig. 2. SEM image of natural magnesite.
Results obtained from EDX (JEOL, JED-2300).
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186 N. Raza et al. / Hydrometallurgy 149 (2014) 183–188

Fig. 3. Effect of temperature on leaching of magnesite ore (formic acid concentration, 8%;
particle size, 177–210 μm; stirring speed, 350 rpm; liquid/solid ratio, 14:1 mL/g).
Fig. 5. Effect of liquid/solid ratio on leaching of magnesite ore (formic acid concentration,
8%; particle size, 177–210 μm; stirring speed, 350 rpm; temperature, 65 °C).
as shown in Fig. 7. Considering Arrhenius equation, Eq. (8) can be
expressed as:

For the chemically controlled reaction, 1=3 −Ea=RT

1−ð1−xÞ ¼ ko e t ð9Þ
h i
1=3
t ¼ ko 1−ð1−xÞ ð6Þ
In Eq. (9), Ea is the activation energy and R is the general gas con-
stant. The values of energy of activation and ko are obtained by plotting
For the ash layer diffusion controlled, ln kvs: T1 as shown in Fig. 8. By putting the values of ko and energy of ac-
h i tivation, Eq. (9) can be represented as:
2=3
t ¼ ko 1−3ð1−xÞ þ2ð1−xÞ ð7Þ
1=3 1 −42078=RT
1−ð1−xÞ ¼59:41  10 e t ð10Þ
Statistical and graphical methods were applied to test the soundness
of the experimental data. It was inferred that the experimental results
for the dissolution reaction of magnesite follow a surface chemical reac- The value of activation energy (42.08 kJ mol−1) depicts that the dis-
tion. The integral rate for the surface chemical reaction can be expressed solution process of natural magnesite in formic acid solution is a chem-
as: ically controlled reaction and this value is in accordance with the results
described in the published research studies (Ashraf et al., 2005; Demir
1=3
1−ð1−xÞ ¼kt ð8Þ et al., 2003; Lacin et al., 2005).
In order to find the validation of the kinetic model (Eq. (10)), exper-
Using the conversion values for various reaction temperatures, the imental conversion values and calculated conversion values for magne-
apparent rate constant k, is determined by plotting 1 − (1 − x)1/3vs. t site were plotted and the results are shown in Fig. 9. From the scatter
diagram (Fig. 9), it can be seen that the correlation of the experimentally
determined conversion values and calculated conversion values is good

Fig. 4. Effect of formic acid concentration on leaching ore (particle size, 177–210 μm; stir- Fig. 6. Effect of particle size on leaching of magnesite ore (formic acid concentration, 8%;
ring speed, 350 rpm; liquid/solid ratio, 14:1 mL/g; temperature, 65 °C). stirring speed, 350 rpm; liquid/solid ratio, 14:1 mL/g; temperature, 65 °C).
 Author's Personal Copy
N. Raza et al. / Hydrometallurgy 149 (2014) 183–188
Fig. 7. Plot of 1 − (1 − x)1/3 and 1/t.
and the value of correlation coefficient (0.9862) of this agreement also
reveals that the workability of the kinetic model is good.
5. Conclusions
• Organic acids can be used as attractive solvents for selective leaching
and beneficiation studies for various rocks as these acids have some
advantages over the mineral acids.
• The results indicate that formic acid can be employed as a solvent for
leaching of magnesite. A formic acid concentration of 8% with a liquid/
solid ratio of 14:1 mL/g was found to be promising for the leaching of
magnesite.
• The kinetic data analyzed on the basis of different reaction kinetic
models illustrates that the dissolution process of natural magnesite
in formic acid is controlled by surface chemical reaction. The energy
of activation of the leaching reaction is 42.08 kJ mol−1.
• In the dissolution reaction of magnesite in formic acid solution, the
reaction product formed (magnesium formate) can be used in various
animal feed formulations as well as in various more general chemical
applications.
Fig. 8. Plot of lnk and 1/T.
187
Fig. 9. Agreement between experimental conversion values and calculated conversion
values of magnesite.
Explanation of symbols
Ea activation energy (J mol−1)
t reaction time (min)
T reaction temperature (K)
EDX energy-dispersive X-ray analysis
SEM scanning electron microscope
AAS atomic absorption spectrophotometer
Acknowledgement
The authors are grateful to the anonymous reviewers for their con-
structive comments and improvement to the manuscript. The authors
also thank the Institute of Chemical Sciences, B.Z.U., Multan for provid-
ing the facilities.
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