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Powder Technology 301 (2016) 1016–1024

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Powder Technology

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Beneficiation studies of a difficult to treat iron ore using conventional and


microwave roasting
Swagat S. Rath a,⁎, Nikhil Dhawan b, D.S. Rao a, B. Das a, B.K. Mishra a
a
CSIR-Institute of Minerals and Materials Technology, Bhubaneswar 751013, India
b
Indian Institute of Technology, Roorkee 247667, India

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

Article history: This work illustrates the reduction roasting and magnetic separation studies of a complex Indian iron ore with
Received 20 January 2016 57% Fe that could not be upgraded to N 61% Fe using a flow sheet comprising of the conventional unit operations
Received in revised form 4 July 2016 like scrubbing, jigging, magnetic separation or flotation. The sole reason of the poor response to physical benefi-
Accepted 20 July 2016
ciation was mainly attributed to the inadequate liberation of iron as visualized under the reflected light micro-
Available online 22 July 2016
scope, which revealed the fine dispersion of silica particles within the hematite grains and vice versa. In order
Keywords:
to overcome this problem, the ore was subjected to reduction roasting using conventional as well as microwave
Reduction roasting heating followed by magnetic separation. The effects of different process variables such as reductant concentra-
Microwave tion, time, and temperature during the process of roasting were studied and subsequently optimized using the
Iron ore Taguchi statistical design. Optical microscopy and X-ray diffraction (XRD) studies of the roasted mass confirmed
Taguchi design the formation of magnetite with simultaneous disappearance of the hematite and goethite phases. In the micro-
Magnetic separation wave roasting process, the reduction could be achieved in a considerably shorter time as compared to the con-
ventional roasting, and the formation of undesired non-magnetic iron minerals like fayalite was limited as
well. In both the processes, it was possible to achieve an iron ore concentrate having 63–65% Fe accompanied
by ~85–90% weight recovery.
© 2016 Elsevier B.V. All rights reserved.

1. Introduction [6] have presented a detailed review of the classical and basic research
work done in this regard. Recently, Li et al. [7] proposed a methodology
The processing and utilization of iron ores are intimately linked to for utilization of low-grade iron ore tailings by the roasting and magnet-
their mineralogical characteristics, liberation pattern, and the nature ic separation technique. Similarly, using a similar strategy, low-grade
of inclusion of the impurities such as SiO2, Al2O3, P and S. The goethitic, oolitic iron ores containing 30–45% Fe could be upgraded to an iron
oolitic and wad type ores containing high silica and alumina are very ore concentrate assaying 58–62% Fe with reasonable recoveries [8].
difficult to process by conventional beneficiation techniques. The bene- Very recently, the coupled approach of reduction roasting and magnetic
ficiation of low-grade ores particularly with a complex mineralogical as- separation was applied to a low-grade iron ore with 51.3% Fe, which
sociation of iron with silica and alumina particles is a challenging produced an iron ore concentrate of 63.3% Fe at 79% recovery [9]. In an-
proposition to all mineral scientists. Thus, many iron ore deposits of other investigation, iron minerals could be converted directly to a me-
India require alternate beneficiation approaches to produce an accept- tallic iron concentrate of 89.63% Fe with 96.21% recovery at a higher
able feed for iron and steel making. temperature of 1250 °C using coal as a reductant [10]. The reduction
There are a few alternate methods of recovering mineral values from roasting and magnetic separation of a mixture of a low-grade iron ore
complex and difficult to treat ores. Reduction roasting, ultrasonic radia- and siderite could produce an iron concentrate of 61.5% Fe at 91.5% re-
tion and microwave heat treatments are some of the techniques that covery without the addition of any extra reductant [11]. In yet another
have been attempted to recover mineral values from the associated study, a high-quality iron concentrate with 65.97% Fe at a recovery of
gangue particles [1–4]. Reduction roasting followed by magnetic sepa- 92.43% with low phosphorous content could be achieved by adding an-
ration involves the conversion of iron oxides present in the ore to mag- other step of acid leaching after performing reduction roasting [12].
netite. The magnetite thus formed is then suitably recovered by low- Though none of these alternative beneficiation techniques have been
intensity magnetic separation. Iwasaki and Prasad [5] and Uwadiwale implemented successfully on an industrial scale, it is the need of the
hour to conduct extensive pilot scale research and make these processes
feasible for practical applications.
⁎ Corresponding author. Microwave heating is a new area of research in iron ore processing. It
E-mail address: ssrath@immt.res.in (S.S. Rath). is unique and different from conventional heating. Microwave energy is

http://dx.doi.org/10.1016/j.powtec.2016.07.044
0032-5910/© 2016 Elsevier B.V. All rights reserved.
S.S. Rath et al. / Powder Technology 301 (2016) 1016–1024 1017

a non-ionizing electromagnetic radiation with frequencies in the range sample to a very fine size. The chemical analysis of the sample
of 0.3–300 GHz though the frequency range of 2.45 GHz is widely used pertaining to Fe, SiO 2 , Al2 O3 , and loss on ignition (LOI) was
in industries. Microwaves generate molecular motion by migration of determined using the standard methods. The ore contained 57.0%
the ionic species and rotation of the dipolar species. The microwave Fe, 13.0% SiO2, 3.0% Al2O3 and 1.14% LOI. Mineralogical characteriza-
heating of material depends directly on the ratio of the dielectric loss tion of the feed and the roasted products was carried out by optical
and the dielectric constant, also termed as the dissipation factor [13]. microscopy (stereo and reflected light microscope, Leitz, Germany).
The major advantage in microwave treatment is the non-contact energy The X-ray diffraction studies were carried out by a Philips
transfer compared to heat transfer in other processes. Material-selective instrument (PANalytical, X'pert) using Cu-Kα radiation operated at
heating, rapid heating, and volumetric heating are the other advantages. 40 kV and 30 mA.
Hauqe [14] has reported an extensive review on the application of the
microwave energy in mineral treatment processes. Some of the key 2.2. Beneficiation
mineral engineering applications of the microwave are (i) the liberation
of ore with complex mineralogy [15,16] (ii) microwave assisted grind- The iron ore sample was initially subjected to classification, jig-
ing [17] (iii) carbo-thermal reduction of oxide ores [18] and (iv) ging, magnetic separation, and flotation techniques for the recovery
leaching [19]. With the added advantage of the localized and volumetric of the iron values. Magnetic separation studies were conducted by a
heating efficiency of the microwaves, the process kinetics can be signif- laboratory model wet high-intensity magnetic separator (WHIMS)
icantly faster compared to the conventional reduction roasting process. supplied by Box Mag Rapid, England. The magnetic intensity of
It is believed that microwave treatment can enhance the carbo-thermal 7500–16,000 G was applied during the course of the experiments.
phase transformation of hematite ores to magnetite. Unlike convention- Several experiments were carried out by varying the magnetic
al roasting, energy can be saved by avoiding the incidental heating of the intensity and particle size. Reverse flotation studies were carried
gangue material in the ore. Secondly, with specific heating, thermal ex- out at a particle size of below 150 μm using a Denver sub-aeration
pansion of the target mineral will occur resulting in crack formation in flotation machine with a 2 L capacity cell. In these studies,
the gangue matrix that will allow much better liberation of the ore dur- dodecylamine (DDA), soluble starch, and MIBC were used as the
ing grinding. collector, depressant, and frother respectively.
The present work encompasses reduction roasting studies of a
difficult to treat iron ore using conventional as well as microwave
heating. The roasted mass has been subjected to grinding and 2.3. Roasting in the muffle furnace
magnetic separation for obtaining a good iron concentrate. Different
parameters and process levels are studied using the Taguchi All the reduction roasting experiments were carried out in a labora-
statistical design. tory muffle furnace using high-quality refractory crucibles. Activated
charcoal containing 3.0% moisture, 2.5% ash, 1.0% volatile matter and
93.5% fixed carbon was used as the reductant. 500 g of the ore sample
2. Materials and methods (− 10 mm size) was uniformly mixed with a desired amount of the
powdered activated charcoal. The sample was kept inside the furnace
2.1. Sample after setting the desired temperature and holding time. The roasted
sample was immediately water quenched after taking out from the fur-
The low-grade iron ore samples were procured from the iron ore nace. The cooled mass was put into a ball mill and ground to −100 μm
mines of Karnataka, India. The sample was received in lumpy form particle size. The sample was then subjected to low intensity magnetic
and for roasting studies; it was reduced to the desired size by jaw separation (LIMS) having a fixed magnetic intensity of ~ 1800 G. The
crushing followed by roll crushing. The complete chemical analysis magnetic fraction thus obtained was considered as a product while
of the representative sample was carried out after grinding the the nonmagnetic fraction was further subjected to wet high-intensity

Fig. 1. Experimental plan for reduction roasting followed by magnetic separation.


1018 S.S. Rath et al. / Powder Technology 301 (2016) 1016–1024

Table 1 2.5. Taguchi statistical design


Control factors and levels for muffle furnace reduction roasting experiments.

Control factors Levels The roasting experiments were carried out as per the Taguchi exper-
1 2 3 4
imental design in order to optimize the roasting variables for obtaining
the maximum iron grade and recovery. L16 orthogonal arrays were used
A: Roasting temperature, °C 750 850 950 1050
to conduct the four level reductions roasting experiments in the muffle
B: Roasting time, min 30 60 90 120
C: Reductant conc., % 2 4 6 8 furnace. Three factors namely roasting temperature, roasting time, and
reductant concentration were considered while corresponding overall
iron grade and weight obtained from the flow sheet as shown in Fig. 1
were treated as the response variables. The control factors with their se-
Table 2
Control factors and selected levels for the microwave reduction roasting experiments.
lected levels for the experiments are given in Table 1. For microwave
roasting experiments, roasting time, charcoal concentration and particle
Control factors Levels size of the ore were considered as factors and the corresponding Fe
1 2 3 grade and recovery obtained from the process circuit (Fig. 1) were treat-
A: Time, min 2 3 4 ed as the response variables. Accordingly experiments were conducted
B: Charcoal, % 6 8 10 as per the 3 level L9 Taguchi design as explained in Table 2. The software
C: Particle size, mm 1 2 3 MINITAB 14.0 was used for the statistical design and analysis.

magnetic separation (WHIMS) at a magnetic intensity of ~10,000 G. The 3. Results and discussion
magnetic fraction obtained from WHIMS was considered as another
product. The yield and iron grade obtained from the process circuit 3.1. Beneficiation studies
comprising of LIMS and WHIMS were considered as the weight recovery
and grade of the overall process. Initially, experiments were carried out by scrubbing, screening, jig-
ging, and magnetic separation techniques to enrich the iron content of
the ore containing ~57% Fe. Several experiments in each unit were car-
2.4. Microwave roasting ried out to enrich the iron values. The process flow sheet developed in
this regard is shown in Fig. 2. However, it was observed that the maxi-
Microwave assisted reduction roasting experiments were carried mum Fe grade that could be obtained was limited only to 61% Fe with
out using a 2650 MHz domestic microwave oven (LG model MC a weight recovery of 80%. Besides that, reverse flotation studies were
2302FUPG) of 30 L capacity having maximum 900 W of power output. carried out to remove the major impurities such as silica and alumina.
The ore and charcoal mixture were put in a refractory crucible and All the studies were carried out at natural pH (7–7.5), using
placed on the central plate of the oven. The oven was operated at a dodecylamine as the collector (80–100 g/t) and MIBC as the frother
power of 900 W and the temperatures of the test samples were mea- (45 g/t). Here it was possible to achieve a concentrate with 60.8% Fe at
sured quickly by inserting a thermocouple into the sample after the 30% weight recovery only. Although the major impurity in this particu-
power was turned off. The experiments were conducted with 10 g of lar iron ore is silica (13%), the beneficiation studies revealed that it is dif-
ore sample per batch. The overall process of roasting followed by mag- ficult to upgrade this sample to a satisfactory Fe grade. This is mainly
netic separation is depicted in a flow sheet in Fig.1. attributed to its complex mineralogy and textural features.

Fig. 2. Flow sheet for physical beneficiation of the run of the mines ore.
S.S. Rath et al. / Powder Technology 301 (2016) 1016–1024 1019

3.2. Reduction roasting in a muffle furnace

All the roasting experiments were carried out as per the Taguchi
statistical design. The complete results of the muffle furnace
roasting experiments at different conditions are shown in Table 3.
The table includes the iron grade and weight recovery obtained
from LIMS, WHIMS and the combination of the two units as depicted
in Fig. 1. Since, in an orthogonal array, the controlling factors are al-
tered in each experiment, it is difficult to pick the most influential
factor. Therefore, the marginal means of the signal to noise ratios
(S/N ratios) of each factor, which represents the mean S/N ratio for
each factor adjusted for all other variables in the model, plotted
against the factor at different levels are shown in Fig. 4. The ap-
proach was to examine and derive the best performance in terms
of magnitude. As the underlying criteria are maximum iron grade
and recovery, the larger-the-better characteristic was employed. It
is evident that for up to three levels with increasing temperature
and time, the S/N ratio response increases significantly. It is ob-
served that temperature plays the most crucial role followed by
time while charcoal dosage has a comparatively lesser effect over
the range examined. It is clear that the alterations in the parameters
do have a significant effect on the reduction behavior. The overall
best experimental conditions as per the Taguchi design are temper-
ature: 1050 °C, time: 90 min, and charcoal: 4%. Three experiments
were conducted at these conditions, which yielded an overall
grade of ~ 62.5–63%Fe with a weight recovery of ~ 88–90%. This
validates the optimum conditions as determined by the statistical
analysis.
In order to delineate the effect of temperature on phase transfor-
mation, four additional experiments were performed at different
temperatures (750, 850, 950 and 1050 °C) at a fixed charcoal dosage
(4%) and time (90 min), and the corresponding phase changes were
studied mainly by XRD analysis and reflected light microscopy. The
Fig. 3. Reflected light photomicrographs of the feed sample showing (a) extremely fine XRD study of the feed sample (Fig. 5) shows hematite and goethite
silicates within hematite (white) (b) hematite within silicates.
as the iron-bearing minerals and it does not contain any magnetite
mineral. XRD spectra of the roasted samples show the appearance
The sample was subjected to reflected light microscopic studies, of magnetite peaks at the expense/disappearance of hematite
which showed the intricate presence of extremely fine silicate phases peaks with an increase in the roasting temperature. Fayalite peaks
within the hematite phase (Fig. 3(a)). Hematite phases of widely different appear only after 950 °C, whereas wustite appears at 1050 °C. At
shapes and sizes could be observed in the silicates (Fig. 3(b)). This sug- 1050 °C, the spectrum contains more fayalite peaks compared to
gests that the locked arrangement of both iron and silicate phases in the magnetite. Reflected light microscopic studies of the reduced
ore body accounting for the inadequate liberation of the particles. Subse- sample indicate the formation of magnetite, wustite, and fayalite
quently, in order to achieve a better grade and weight recovery, a process at different levels of temperatures (Fig. 6). As a consequence of re-
constituting reduction roasting, grinding, and magnetic separation was duction roasting, magnetite (M) was formed along the borders of
carried out to unlock the structure through phase transformation. the hematite grains with the inclusions of silicates (S). At higher

Table 3
Results of the reduction roasting experiments in the muffle furnace.

Experiment Roasting Roasting Reductant LIMS LIMS WHIMS WHIMS Overall Overall
no. temp time conc. grade, wt., % grade, wt., % wt., % grade,
% % %

1 750 30 2 63.9 4.0 61.2 66.6 70.6 61.3


2 750 60 4 63.4 19.2 59.3 64.2 83.4 60.3
3 750 90 6 63.3 24.0 58.4 57.0 81.0 59.8
4 750 120 8 63.4 34.2 59.3 45.3 79.4 61.1
5 850 30 4 63.9 25.0 59.6 57.2 82.2 60.9
6 850 60 2 62.8 29.0 60.5 52.8 81.8 61.3
7 850 90 8 64.2 53.6 58.6 35.3 88.9 62.0
8 850 120 6 63.7 51.3 58.9 35.4 86.7 61.7
9 950 30 6 55.9 36.1 59.5 50.6 86.8 58.0
10 950 60 8 64.8 16.3 63.9 67.0 83.3 64.1
11 950 90 2 63.4 37.2 61.7 49.5 86.7 62.4
12 950 120 4 63.9 44.2 63.1 40.9 85.1 63.5
13 1050 30 8 66.7 6.5 64.4 70.7 77.1 64.6
14 1050 60 6 66.5 13.3 64.8 68.0 81.2 65.1
15 1050 90 4 65.6 35.9 64.4 51.7 87.6 64.9
16 1050 120 2 64.8 25.2 61.0 52.6 77.8 62.2
1020 S.S. Rath et al. / Powder Technology 301 (2016) 1016–1024

Fig. 4. Taguchi main effects plot for S/N ratios of different factors for the muffle furnace roasting experiments.

temperatures (850 °C), the thickness of the magnetite (M) bands compared to the samples roasted at 950 °C or 850 °C. However,
are found to have increased significantly. As expected, fayalite (F) most of the reduced iron phases get attracted at a higher intensity
occurred above 950 °C, which is in concordance with the XRD of magnetic separation (WHIMS) resulting in a higher overall
results. It can be seen that fayalite is present along the borders of weight recovery.
silicate islands, which suggests the reaction of hematite with
silicates forming fayalite at a higher temperature. Wustite (W) is 3.3. Roasting in microwave oven
present within the borders of the magnetite (M) phase indicating
conversion of magnetite to wustite under appropriate reduction The entire microwave roasting experiments were carried out as
conditions. per the Taguchi statistical design. Three particle sizes of − 3, − 2,
The overall results show that wustite and fayalite are more pre- and − 1 mm were considered for the experimental studies. The ex-
dominant phases at a higher temperature. According to the corre- perimental results obtained from LIMS, WHIMS, and their combina-
sponding ternary phase diagrams of the FeO-SiO2-Al2O3 system, an tion is shown in Table 4. The temperature data recorded for each
ore containing SiO2 will form fayalite at temperatures above 900 ° experiment are also included in the table. The marginal means of
C [20]. This justifies the formation of fayalite in this particular ore S/N ratios were plotted against each factor at different levels and
at high temperatures. Both fayalite and wustite being weakly mag- shown in Fig. 7. The same underlying criteria of maximum iron
netic do not report to the magnetic fraction during the low-intensity grade and recovery, i.e. the larger-the-better S/N ratio, were
magnetic separation of the roasted mass. This explains why the employed. The effects of controllable factors i.e., time, particle
weight recovery in LIMS for the sample roasted at 1050 °C is less size, and charcoal dosage, on the S/N ratio for overall Fe grade/
recovery are shown in Fig. 7. It is evident that with increasing resi-
dence time, the S/N ratio increases significantly. There is an opti-
mum particle size (− 2 mm) and time (4 min) at which the S/N
ratio has the highest response. According to the rank, residence
time followed by particle size and charcoal dosage has the greatest
effect on the process output. Charcoal dosage has a minimal effect
over the range examined. Higher residence time (4 min), medium
particle size (− 2 mm) and low charcoal dosage (6%) represent
the optimal conditions. It is observed that at 4 min of time, the
LIMS grade is found to be ~ 65% Fe with more significant weight re-
covery compared to all other residence times as given in Table 4.
This indicates that the reduced ore gets enriched with magnetite if
treated in the microwave oven for 4 min, irrespective of the char-
coal percentages or particle sizes. However, three experiments
were conducted with the optimum levels of the parameters i.e., res-
idence time: 4 min, particle size: − 2 mm and charcoal percentage:
6%. On an average, a concentrate of 61–61.5% Fe with a weight
recovery of 84–85% could be obtained as a product from the flow
sheet as displayed in Fig. 1.
The phase changes during microwave roasting were studied by
reflected light microscope and XRD analysis. The X-ray diffraction
studies in the case of some selected reduction process are shown in
Fig. 5. XRD patterns of a) feed sample and samples roasted with 6% charcoal, 1.5 h time at
Fig. 8. It is observed that the peak heights of hematite and goethite
b) 750 °C c) 850 °C d) 950 °C e) 1050 °C. H: hematite, M: magnetite, G: goethite, Q: quartz, with respect to the feed are slowly disappearing while new peaks
F: fayalite, W: wustite. of magnetite are appearing as reduction progresses. The appearance
S.S. Rath et al. / Powder Technology 301 (2016) 1016–1024 1021

Fig. 6. Micro photographs of furnace roasted products at (a, b) 750 °C, (c, d) 850 °C, (e, f) 950 °C, (g, h) 1050 °C with 6% charcoal and 1.5 h roasting time. H: hematite (white), M: magnetite
(pinky), F: fayalite, W: wustite, S: silicates (quartz).

of the fayalite peak in some experiments is observed entirely at borders of hematite indicating possible reaction of hematite and
higher residence time and maximum charcoal dosage, whereas the silicates (Fig. 9(e, f)).
wustite peaks do not appear in any of the experiments. Reflected The formation of fayalite takes place only in experiments having
light microscopic studies of the reduced products show a well- higher residence time (N 3 min). It is noteworthy that wustite does
developed magnetite (M) phase indicating conversion of goethite not appear in any of the experiments suggesting that the reduction
and hematite phases (Fig.8). In the roasted product, some silicates conditions such as time and temperature are insufficient for its for-
(S) enclosed within the hematite phase are seen. The coaly matters mation as against the conventional reduction roasting experiments.
(C) as observed within the reduced samples (Fig. 9(a, b)) are the un- According to the corresponding ternary phase diagram of the iron
used carbon present, because of the insufficient time of microwave oxide system, wustite cannot form below 570 °C [21], and in all
roasting. Fayalite is observed in the silicate matrix alongside the nine experiments the highest temperature recorded was around
1022 S.S. Rath et al. / Powder Technology 301 (2016) 1016–1024

Table 4
Reduction roasting in the microwave oven.

Experiment Time, Charcoal, Particle LIMS LIMS WHIMS WHIMS Overall Overall Temp,
no. min % size, grade, wt., grade, wt., % wt., % grade, °C
mm % %, % %

1 2 6 −3 64.2 5.4 62.2 83.3 84.2 62.3 380


2 2 8 −2 65.3 10.4 62.6 82.1 84.0 62.9 492
3 2 10 −1 65.3 7.7 64.2 75.9 77.7 64.3 364
4 3 6 −2 65.2 45.8 58.6 82.1 90.3 61.9 520
5 3 8 −1 64.6 47.0 56.7 85.2 92.1 60.7 557
6 3 10 −3 65.6 47.9 57.7 82.8 91.0 61.9 522
7 4 6 −1 64.2 60.9 58.5 71.7 88.9 62.4 556
8 4 8 −3 63.9 54.9 58.5 78.8 90.5 61.8 517
9 4 10 −2 65.1 50.0 58.4 83.3 91.7 62.0 533

Fig. 7. Taguchi main effects plot for S/N ratios of different factors for the microwave roasting experiments.

566 °C. The carbon monoxide formed during the microwave roasting essentially retained the heat longer than the smaller particles thereby
could facilitate the formation of magnetite. However, a higher showing enhanced reduction. The reduction of fayalite is more difficult
amount of fayalite and wustite could not be formed. Moreover, compared to wustite [22] for which no commercial process has yet been
during furnace roasting experiments, a coarser particle size was developed. Therefore, having less fayalite in the microwave reduced
used as compared to the microwave roasting experiments, which product is an advantage.

4. Conclusion
(e)
An iron ore with 57% Fe was found to be unresponsive to conven-
tional beneficiation techniques because of the inherent complex
(d) mineralogy pertaining to fine-grained silica particles that are locked
within hematite grains. A different approach based on reduction
roasting and microwave heating followed by magnetic separation
(c) was considered to reduce and recover the iron values. The effects
of different process parameters in both cases were analyzed using
the Taguchi statistical design. The furnace roasting route yielded
an iron concentrate of ~ 63–64% Fe at ~ 88–90% weight recovery
(b)
while the microwave roasting yielded ~ 62–63% Fe at ~ 84–85%
weight recovery. The change in mineralogical composition in both
the cases was studied through reflected light microscopy
accompanied by XRD analysis. The overall weight recovery obtained
(a) through the process comprising reduction roasting followed by two
stages of magnetic separation (LIMS and WHIMS) were very similar
for both the routes. However, the results of microwave roasting
showed that it has a tremendous potential to produce an equally
Fig. 8. XRD patterns of sample roasted in microwave oven (a, b, c, d and e refer to feed, exp.
good roasted product in a much lesser time period accompanied
no. 3, 7, 8 and 9 respectively). H: hematite, M: magnetite F: fayalite, G: goethite; F: fayalite, by a lesser formation of undesired products like fayalite, which is
W: wustite, Q: quartz. an added advantage.
S.S. Rath et al. / Powder Technology 301 (2016) 1016–1024 1023

(a) (b)

C H M
C
M
(c) (d)
C
S H
H
S
C M
(e) (f)

M
H M

(g) (h)

H M
F S H
S

Fig. 9. Photomicrographs of microwave roasted samples (a, b) Experiment 1, (c, d) Experiment 2, (e, f) Experiment 6, (g, h) Experiment 7. The experiment numbers correspond to Table 4.
H: hematite (white), M: magnetite (pinky), F: fayalite, C: carbon, S: silicates (quartz).

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