International Journal of Mineral Processing 87 (2008) 120–128

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International Journal of Mineral Processing

j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / i j m i n p r o

Kinetics of thermal decomposition of Hekimhan–Deveci siderite ore samples

Dilek Alkaç ⁎, Ümit Atalay
Mining Engineering Department, Middle East Technical University, Ankara, Turkey

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

Article history: Different solid-state reaction models, by interpretation of the model graphs in terms of goodness of fit to real
Received 5 June 2007 data points (R-squared), are used to evaluate the reaction mechanism and the kinetics (E, n) for the thermal
Received in revised form 17 February 2008 decomposition of Hekimhan–Deveci siderite ore samples. Isothermal experiments at three different
Accepted 22 February 2008
temperatures (T = 505 °C, 520 °C, 535 °C) are run for t = 15–150 minutes while non-isothermal experiments
Available online 29 February 2008
are conducted at single heating rate (10 °C/min) using thermogravimetric analysis (TGA). Three-dimensional
diffusion reaction models have been noted as the solid-state reaction model representing thermal
Keywords:
decomposition kinetics of Hekimhan–Deveci siderite. The values of activation energy (E), the optimum
Siderite ore
kinetics obtained, are E = 85.53 kj/mol (Jander three-dimensional diffusion reaction model); E = 85.49 kj/mol,
Three-dimensional diffusion model
Activation energy (Ginstling–Brounshtein three-dimensional diffusion reaction model).
© 2008 Elsevier B.V. All rights reserved.

1. Introduction due to dissociation of FeCO3 at temperature range of 475–540 °C and

Thermal treatment processes, endothermic in nature, result in
thermal decomposition, phase transition, driving-off the volatile
fraction depending on the type of ore treated and experimental
conditions. Carbonate minerals (CaCO3, MgCO3, CuCO3, MnCO3, FeCO3
etc.) are of interest in respect to thermal decomposition characteristics
and products obtained at the end of the process; thermal decomposi-
tion, calcination, takes place below the melting point of the mineral
when heated. Thereafter, oxidation reactions result in formation of
new species, having differences in characteristics.
Endothermic and exothermic reactions taking place in thermal
decomposition process yield transformations; being paramagnetic at
room temperature, siderite is converted to ferromagnetic and
ferrimagnetic phases upon controlled heat treatment. Thus concen-
tration by low-intensity magnetic separation is enhanced, eliminating
the need of high-intensity magnetic separation, which is compara-
tively more expensive and complex. Determination of temperature
range of operation is critical for achievement of obtaining phases
readily concentrated by low-intensity magnetic separation. Gaseous
atmosphere, in which thermal decomposition reactions take place,
affects the final product characteristics.
The decomposition of siderite has been studied in a number of
gaseous atmospheres; under the flow of oxygen it is found that, the
oxidation is so rapid that the only detectable phase as the end product
is hematite, α-Fe2O3, while magnetite, Fe3O4 and wüstite, FeO, are
observed in vacuum or in an inert atmosphere.
The theoretical data on decomposition of siderite points out that,
siderite has a characteristic thermal curve with endothermic effect
⁎ Corresponding author. Tel.: +1 801 581 6309; fax: +1 801 581 4937.
E-mail address: dalkac@gmail.com (D. Alkaç).
subsequent exothermic effect, corresponding to oxidation of FeO.
It has been reported that particle size of the ore, quantity of
sample, and pressure are effective on thermal decomposition, as well
(Dhupe et al., 1990; Gotor et al., 2000).
Specifically the effect of particle size on thermal decomposition has
been the subject of the studies of Jagtap et al. (1992); various particle
sizes have been treated at different temperatures and heating rates
under isothermal and non-isothermal conditions respectively. The con-
clusion has been in the way that the mechanism of thermal decom-
position of siderite is the same for all particle sizes studied, emphasizing
the importance of experimental conditions (Jagtap et al., 1992).
As the chemical composition of the ore has been found effective in
analyzing the kinetics of thermal decomposition of siderite, since
magnesium (Mg), calcium (Ca), and manganese (Mn) may substitute
for iron (Fe) in siderite ore, there are a number of studies conducted to
investigate the kinetics; Kubas and Szalkowicz (1971) have calculated
the activation energy of decomposition by model-free method.
Zakharov and Adonyi (1986) have employed n-order kinetic model
to calculate kinetic parameters. Avrami Erofe'ev has been validated as
Table 1
Chemical composition of Hekimhan–Deveci siderite ore
%
Fe 37.69
MgO 2.86
Al2O3 1.36
CaO 1.39
MnO 5.54
SiO2 5.67
Loss on ignition 28.87

0301-7516/$ – see front matter © 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.minpro.2008.02.007
 D. Alkaç, Ü. Atalay / International Journal of Mineral Processing 87 (2008) 120–128 121

Fig. 1. TGA of Hekimhan–Deveci siderite ore, in air atmosphere at heating rate of 10 °C/min.

Fig. 2. DSC analysis of Hekimhan–Deveci siderite ore at T = 50 °C–600 °C.

Fig. 3. Results of laboratory heating experiments, t = 15–45 min.

122 D. Alkaç, Ü. Atalay / International Journal of Mineral Processing 87 (2008) 120–128
the model interpreting the kinetic behavior of thermal decomposition
of siderite (Gotor et al., 2000). Obtained parameters have been shown
to be different since all researchers conducted thermal decomposition
reaction experiments using different chemical compositions, under
presence of different gases.
Samples having the lowest siderite content (72% by weight) were
studied in vacuum by Kubas and Szalkowicz, and a value of 115 kJ/mol
was noted as the activation energy of thermal decomposition,
determination of mechanism of the process was conducted as well
in studies of Zakharov and Adonyi, Dhupe and Gokarn, Jagtap et al.
Among all, the highest value of activation energy was found in study,
carried out under nitrogen flow, of Zakharov and Adony (E = 238 kJ/
mol). Avrami Erofe'ev reaction mechanism was pointed out to be
descriptive of thermal decomposition kinetic of siderite, under air at-
mosphere, in the studies of Dhupe and Gokarn (E=41 kJ/mol) and Jagtap
et al. (E =77 kJ/mol).
The thermal decomposition of mineral siderite (FeCO3), an iron
bearing carbonate mineral which on calcination converted to iron
oxide (α-Fe2O3 or γ-Fe2O3 or Fe3O4) during the process, has been
studied in detail due to industrial relevance of the final product, i.e. in
supply of raw material for blast furnaces or in flue gas desulphuriza-
tion (Atesok et al., 2000; Jagtap et al., 1992; Böhm et al., 2006).
Owing to the properties of calcined products, such as high pore
volume and high surface area, the end products are also used in
capture of sulphur dioxide (SO2) in a wide temperature range.
Scarce of high grade iron ore, qualifying as the feed to blast furnace,
is the problem of industry in Turkey. The recovery obtained by
smelting in blast furnace via which iron is obtained in metal form, is
diminished consequently. Fortunately, there are studies conducted
with the aim of handling the problem; in a pilot study, siderite ore has
been treated in rotary furnace, yielding products high in iron grade
(Atesok et al., 2000).
However, considering that industrial applicability is sought
principally, it is essential that the process conditions are improved
extensively. Practicality of application, to some extent, is dependent
on use of or modification of current technology on economical basis.
Therefore, reactions taking place in air atmosphere are of interest,
Fig. 4. DTA of Hekimhan–Deveci siderite ore, in air atmosphere at heating rate of 10 °C/min.
remarking that not only obtaining phases high in iron grade but also
responsive to low-intensity magnetic separation is required.
As an extension of the investigation of thermal treatment of
Hekimhan–Deveci siderites to obtain phases showing high magnetic
susceptibility (γ-Fe2O3 or Fe3O4) by microwave heating, this work has
been focused on the thermal decomposition characteristics of the ore.
Microwave heating experiments have not yielded magnetic phases as
expected (Znamenackova et al., 2005; Böhm et al., 2006), even tough
high magnetic susceptibility phases could be obtained under
controlled conditions (temperature, T–time, t) by conventional
heating. Showing differences in microwave heating profile, Hekim-
han–Deveci siderite ore has been thought to follow a different thermal
decomposition mechanism. Thus the objective of the present study is
to analyze detailed thermal decomposition of Hekimhan–Deveci
siderite ore, by checking the consistency of data by available models.
The results of models, which represent the data adequately, have been
given taking into account that there are many factors influencing
thermal decomposition in respect of kinetics.
In isothermal experiments, run-of-mine (r.o.m.) ore sized down to
−20 mm was used while −75 μm was used in non-isothermal runs for
TGA; heat treatment of different sizes did not influence the kinetic
parameters, in agreement with the results of previous studies [Jagtap
et al. (1992)]. Samples have been prepared under same conditions and
heating experiments were conducted in identical experimental
conditions.
The results of TGA interpreted by computational methods have
been relied upon in estimation of the apparent overall kinetics
parameters, analysis for siderite thermal decomposition kinetics has
been based solely on TGA results in literature (Gotor et al., 2000;
Dhupe et al., 1990; Jagtap et al., 1992; Sanders and Gallagher, 2003).
However, the fact that conducting the experiments in such a way
may not go beyond the simulation of conventional heating, is a
matter of question and it is remarked that effect of experimental
conditions, which may be well observed in laboratory scale set up,
on reactions is important; therefore in present work the objective has
been obtaining consistent parameters, putting weight on the sur-
rounding conditions.
 D. Alkaç, Ü. Atalay / International Journal of Mineral Processing 87 (2008) 120–128 123

2. Experimental for identification of thermal decomposition profile of the ore. Thermogravimetric

2.1. Materials and methods
Malatya (Hekimhan–Deveci) siderite ore was used as the material subjected to heat
treatment in the study. The chemical composition of the ore has been determined by X-
ray fluorescence (XRF) analysis and the results are as shown on the following table
(Table 1). The XRD pattern of the ore indicated that siderite is the main mineral;
ankerite (CaFe(CO3)2), dolomite (CaMg(CO3)2), calcite (CaCO3), quartz (SiO2), hematite
(α-Fe2O3) were also determined to be present within the ore. Verified ore composition
has been revealed in microscopical examination.
Taking account of the fact that achievement of indicated goal is dependent on
setting temperature range of operation, thermal analyses have been referenced in order
analysis (TGA) at temperature range of 25 °C–900 °C, differential thermal analysis (DTA)
at temperature range of 25 °C–900 °C were conducted while differential scanning
calorimetry analysis (DSC) analysis was conducted at a range of 50 °C–600 °C
respectively. Set of heating experiments were carried out on laboratory scale to decide
on the range of data collection for isothermal heating runs. The fact that it is almost
impossible to rely on significance of time since, at high temperatures, weight loss of
samples takes place at higher rate on continuous heating. Therefore the limits of
operation range were determined in light of results of thermal analyses and
experimental work. Laboratory heating experiments have subsequently followed the
TG analysis to get the data with respect isothermal heating, referencing the theoretical
data on thermal decomposition of siderite. Noting “time” as the parameter that
determines the conversion at any point on isothermal runs, samples, −20 mm, have

Fig. 5. XRD analysis of Hekimhan–Deveci siderite ore on samples.

124 D. Alkaç, Ü. Atalay / International Journal of Mineral Processing 87 (2008) 120–128

Table 2 The expression for fractional conversion with respect to time in isothermal
Solid-state reaction models (Gotor et al., 2000; Dhupe et al., 1990; Mamleev et al., 2000) experiments, and on basis of temperature in non-isothermal experiments is;
and results obtained through analysis
ðsamplemassÞj
Reaction model f(x) n (reaction order) E (kj/mol) R2 x¼  100 ð1Þ
ðsamplemassÞinitial
1/n
1. Power law (x)
n = 1.0051 32.58 0.792 j = particular time (minutes) or particular temperature (˚C)
n = 1.0437 30.85 0.787 Initial Temperature = 25˚C
n = 1.1911 25.30 0.763
2. Exponentional law ln(x) 2.2. Kinetic analysis
3. Avrami Erofe'ev [−ln(1 −x)]1/n
nN1 Kinetic parameters determined in this study are reaction order and activation
n = 1.086 35.25 0.811 energy along with the reaction mechanism. Calculations on isothermal runs are based
n = 1.1215 33.71 0.807 on Eq. (2);
n = 1.2603 28.45 0.790
4. Prout–Tompkins ln[x/(1 − x)] f ðxÞ ¼ kðT Þ  t ð2Þ
5. One-dimensional x2
Diffusion t = time (minutes)
6. Two-dimensional (1 − x)ln(1 − x) + x T = temperature (Kelvin, K)
diffusion
7. Jander three- [1 − (1 − x)1/3]2 85.53 0.860 Expressions for f(x), reaction model, comprise of the particular fractional
dimensional diffusion conversion and related mechanism in terms of mathematical equations; once the
8. Ginstling–Brounshtein [1 − (2x/3)] − (1 − x)2/3 85.49 0.858 fractional conversion with respect to time, x vs. t, data is obtained by isothermal
three-dimensional experiments the calculation of f(x) values for given conversions is straight forward. The
diffusion linearity of line of data plotted, f(x) vs. t, is indicator of the degree of fit; the slope gives
9. Geometric models 2[1 − (1 − x)1/2] the value of rate constant, k, at temperature of interest.
(contracting area) Kinetic parameters determination in non-isothermal runs has been through Eq. (3);
10. Geometric models 3[1 − (1 − x)1/3]
(contracting volume)

AR E
11. Order of reaction −ln(1 − x) ln½f ðxÞ  2lnðT Þiln  ð3Þ
Eb RT
models (n = 1)
12. Order of reaction (1 − x)− 1 E = Activation Energy, kJ/mol
models (n = 2) T = temperature (Kelvin, K)
−2
13. Order of reaction (1 − x)
models (n = 3)
As defined by Eq. (3), the value of (E/RT) is obtained by the slope of line of
{ − [ l n f (x)] vs. (1/T )} the degree of linearity of the line also verifies the consistency of
the model in representing the data. Eventually activation energy, E, is calculated by
multiplication of the value of slope with universal gas constant, R [R = 8.314J/mol × K].
been heated at various temperatures for time periods. Conventional heating, in muffle In addition, conventional method of calculation of E is by use of Arrhenius Eq. (4).
furnace namely PROTHERM, has been method of heat treatment in isothermal
experiments. The applied temperatures are T = 505 °C, 520 °C, 535 °C in range of kðT Þ ¼ ko  expðE=RT Þ ð4Þ
t = 15–150 min. The calcination point, the point at which the mass of sample becomes
almost constant on further heating, for each temperature is the end point of heating Rearrangement of the equation in exponentional form yields;
process. The fractional weight loss data, x, has been found using the results of
experiments and related mathematical equations. lnðkÞ ¼ lnðkoÞ  E=RT
TG analysis has been the method of acquiring the data of heating profile on basis of
increasing temperature against time. The obtained data has been used in analyzing The slope of the plot −lnk vs. (1/T) gives (E/R), thus comparison of values obtained
heating characteristics of material on non-isothermal scale. The data of sample mass both in isothermal and non-isothermal runs for the reaction model of interest becomes
against temperature recorded by “Perkin Elmer Pyris 1 TGA” instrument has been used possible, reporting to be a good method of checking the consistency. On calculations, k
in calculation of conversion for non-isothermal runs. values have been obtained by the slopes of plots (f(x) vs. t) in isothermal runs; taking

Fig. 6. Fractional conversion data evaluated by Avrami Erofe'ev Reaction Model vs. ln(t) for determination of reaction order (n) values [3rd reaction model in Table 2].
 D. Alkaç, Ü. Atalay / International Journal of Mineral Processing 87 (2008) 120–128 125

Fig. 7. Fractional conversion data evaluated by Power Law Reaction Model vs. ln(t) for determination of reaction order (n) values [1st reaction model in Table 2].

Fig. 8. Jander Three-dimensional Diffusion Model (Diffusion Model I) evaluated on basis of fractional conversion values (x) at different temperatures vs. time [7th reaction model in Table 2].

Fig. 9. Ginstling–Brounshtein Three-dimensional Diffusion Model (Diffusion Model II) evaluated on basis of fractional conversion values (x) at different temperatures vs. time [8th
reaction model in Table 2].
126 D. Alkaç, Ü. Atalay / International Journal of Mineral Processing 87 (2008) 120–128

Fig. 10. Avrami Erofe'ev Reaction Model evaluated at different conversion values (x) at respective orders indicated vs. (1000/T).

Fig. 11. Power Law Reaction Model evaluated at different conversion values (x) at respective orders indicated vs. (1000/T).

Fig. 12. Diffusion Reaction Models evaluated at different conversion values (x) vs. (1000/T).
 D. Alkaç, Ü. Atalay / International Journal of Mineral Processing 87 (2008) 120–128
Fig. 13. Evaluation of results of heating experiments, using Ink values obtained by graphs of diffusion reaction models (Figs. 8 and 9), by Arrhenius Relation.
the natural logarithm of k values gotten for constant temperature of concern, the data
for evaluation by Arrhenius equation is gained.
3. Results and discussion
Results of thermal analyses have given close insight to thermal de-
composition profile of ore samples, along with the laboratory ex-
periments. Characteristic TGA curve has indicated that thermal
decomposition starts at around T = 465 °C and also that thermal de-
composition is significant at temperature range of 465 °C–550 °C (Fig. 1).
Range of process of interest has been demonstrated by DSC curve (Fig. 2)
as well; endothermic peak of thermal decomposition is confirmed to be
at T = 525 °C.
In conjunction with thermal analyses, experimental work has justified
the temperature range of thermal decomposition, based on time (Fig. 3).
Thermal decomposition characteristics of Hekimhan–Deveci siderite
ore samples have been verified by differential thermal analysis (DTA)
(Fig. 4).
Decomposing according to the reaction, Hekimhan–Deveci siderite ore
undergoes oxidation reactions commencing at 560 °C up to 650 °C;
thereafter there is no significant reaction observed by DTA curve.
Endothermic heat flow at 650 °C–750 °C may be described by thermal
decomposition of other carbonate minerals present (MnCO3 and MgCO3)
in the composition.
FeCO3 →FeO þ CO2
Subsequent to decomposition of iron carbonate, oxidation reactions
take place in the system, under presence of air; possible set of reactions is
as given below,
4FeO þ O2 →2γ  Fe2 O3
6FeO þ O2 →2Fe3 O4
4FeO þ O2 →2α  Fe2 O3
Characterization of phases present, both for untreated samples and end
products of heat treatment, have been accomplished through X-ray
diffraction (XRD) analysis. Qualitative examination has verified formation
of magnetic phases (ferromagnetic or ferrimagnetic); illustration of
analyses results has been given for selected temperatures (Fig. 5).
What is more magnetic susceptibility analyses proved valid as means
of checking achievement of basic goal, that is obtaining phases that would
respond to low intensity yielding values of mass magnetic susceptibility of
846⁎10− 8 m3/kg at 465 °C, 3721.4⁎10− 8 m3/kg at 510 °C, 18,253.3⁎10− 8 m3/kg
at 560 °C respectively as the result of treatment of the sample
127
which has originally a mass magnetic susceptibility of 92⁎10− 8 m3/kg at
25 °C.
Kinetic models for solid-state reactions (Table 2) have been tested for
ore of interest by consideration of all factors stated. The criterion, in
assessing the model validity with respect to recorded data, has been the
consistency of graphical representation of data both for isothermal and
non-isothermal runs. Thereby, Avrami Erofe’ev, Power law, and Diffusion
(2) reaction models have been found to represent the thermal decom-
position data obtained by experiments. The results of kinetic parameter
analysis, by all four methods, indicated are presented (Figs. 6–13), data
from isothermal and non-isothermal runs have been examined as
discussed in experimental section. Summary of parameter values obtained
through analysis are included on the table for indicated reaction models.
The reaction models being in origin sigmoid rate equation (3rd reaction
model; Table 2), acceleratory rate equation (1st reaction model; Table 2),
and deceleratory rate equations (7th and 8th reaction models; Table 2)
respectively diffusion reaction models have better fit. Therefore, diffusion
reaction models, specifically 3-D, are concluded to be models defining the
thermal decomposition kinetics among all solid-state reaction models.
In agreement with the outcome of the isothermal runs, adequacy of the
diffusion reaction models in representing the data has been confirmed by
non-isothermal runs. The best degree of fit value (R2) belongs to 3-D
diffusion reaction models.
By use of Arrhenius equation in evaluating the data for isothermal
runs, activation energy (E) values have been determined on basis of
ð5Þ 7th and 8th reaction models in Table 2. The figure (Fig. 13) shows
the determination of E by Arrhenius relation in terms of graphical
representation.
Examination of results in terms of degree of fit brings about the
conclusion that three-dimensional diffusion models are the reaction
ð6Þ models representing the thermal decomposition kinetics of Hekimhan–
Deveci siderite ore. In contrast to the study (Dhupe et al., 1990), the
ð7Þ experimental data obtained from Hekimhan–Deveci siderite ore proves to
have a better fit to 3-D diffusion models rather than the Avrami–Erofe’ev
ð8Þ
model.
Type of ore treated reports to be the reason explaining the difference in
results; furthermore consistency of diffusion models in describing the
Table 3
Kinetic parameters of diffusion reaction models
Isothermal runs Non-isothermal runs
Activation energy (E) (kj/mol)
Diffusion Model I 85.53 93.96
Diffusion Model II 85.49 106.85
128 D. Alkaç, Ü. Atalay / International Journal of Mineral Processing 87 (2008) 120–128
kinetics have also been verified by influence of parameters such as
chemical composition or temperature range operated.
Reaction models determined for the process are;
Three-dimensional Diffusion Model (Diffusion Model I):
h i
f ðxÞ ¼ 1–ð1–xÞ1=3 2
Ginstling–Brounshtein Diffusion Model (Diffusion Model II):
f ðxÞ ¼ ½1–ð2x=3Þ–ð1–xÞ2=3 :
Evaluation of model equations via Arrhenius relation gives comparable
results for activation energy, indicative of the fact that the reaction is
diffusion controlled in set conditions (Table 3).
Consequently it is seen that not only the results are precise within
identical runs, i.e. isothermal or non-isothermal runs, but also consisten-
cy is observed among different runs, as expected. Anyhow, under any
circumstances, influence of experimental conditions and of the studied
range as well as the characteristics of material must be accounted in
analyzing the results.
4. Conclusion
Hekimhan–Deveci siderite ore has a characteristic thermal curve,
on which intense heat flow to the system, corresponding parts of
endothermic reactions, is required in the first place. Exothermic
reactions take place following the thermal decomposition, generating
heat through the system. Calcination process has been shown to have
all effects cited, i.e. thermal decomposition, driving-off volatile ma-
terial (CO2 in the case) and phase transition, on heat treatment of the
ore. In accordance to the solid-state reaction models which are
classified into subclasses, with respect to the mechanism, that either
the rate is acceleratory or deceleratory, the present study has con-
cluded that thermal decomposition is represented by diffusion reac-
tion models, particularly three-dimensional diffusion models.
Models of three-dimensional diffusion, Three-dimensional Dif-
ð9Þ fusion Model and Ginstling–Brounshtein Diffusion Model, give iden-
tical results by different methods; reliability of findings is thereby
verified. On the other hand, it is noteworthy to emphasize that the
decomposition of siderite is influenced by conditions of treatment, and
ð10Þ
also by the substitutions in chemical composition.
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