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Improving coke strength prediction using automated coal petrography

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 Fuel 94 (2012) 368–373

Contents lists available at SciVerse ScienceDirect

Fuel
journal homepage: www.elsevier.com/locate/fuel

Improving coke strength prediction using automated coal petrography

Sushil Gupta a,⇑, Fenglei Shen a, Woon-Jae Lee b, Graham O’Brien c
a
Center for Sustainable Materials Research & Technology, School of Materials Science and Engineering, The University of New South Wales, Sydney, NSW 2052, Australia
b
POSCO Technical Research Laboratory, Pohang City, Gyeongbuk, Republic of Korea
c
CSIRO Earth Science and Resource Engineering, QCAT, Brisbane, Australia

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

Article history: A range of Australian and overseas coals with a mean maximum vitrinite reflectance (Ro, max) range of
Received 29 April 2011 0.68–1.71% were carbonized in a test coke oven. Coal properties were characterized using XRF, XRD and
Received in revised form 20 September automated imaging of polished sections of discrete coal grains. The Full Maceral Reflectance (FMR) param-
2011
eter was calculated from the reflectance data and was correlated with coal as well as coke properties. The
Accepted 21 September 2011
Available online 5 October 2011
Ro, max values and the vitrinite estimates from the semi-automated microscopic technique indicated a
good correlation with similar data based on manual point count analysis. The FMR parameter is shown
to increase with increasing carbon content, structural ordering of carbon and decrease with increasing vol-
Keywords:  
Coal atile matter. The FMR parameter of coal was related to cold coke strength DI15015 and coke strength after
Reflectogram reaction (CSR). The FMR parameter was modified by diluting the contribution of high reflectance coal grains
Microscopy
as well as incorporating the effect of ash contribution to propose a combined coal index (CCI). The new coal
Full maceral reflectogram
CSR and DI
index is shown to improve the accuracy of coke strength prediction. The combined coal index provides a
promising objective measurement based alternative for predicting coke strength.
Ó 2011 Elsevier Ltd. All rights reserved.

1. Introduction characteristics. One of the popular models is the Schapiro model,

Coal composition is popularly characterized in terms of macerals
which are the microscopically recognizable individual constituents
of coal. On the basis of their quantitative participation and associa-
tion, macerals determine the chemical and physical properties of a
given coal. Coal macerals are divided in three groups: vitrinite, lipt-
inite (or exinite) and inertinite and is distinguished by the propor-
tion of light reflected from the surface of a polished specimen
surface. Due to overlap of reflectance between the macerals, mor-
phological features are also used for the identification [1]. Generally,
vitrinite is the most abundant group in high rank coals and its reflec-
tance is usually less than that of inertinites but greater than liptinites
[2]. Inertinite displays highest reflectance and varies significantly
among different coals, and characterized by highest carbon content
mostly in aromatic form, least volatiles components including
hydrogen [3]. Generally, inertinites remain inert during carboniza-
tion with the exception of some Australian coals inertinite [4].
Coke strength is critical for ironmaking via blast furnace route
and is strongly influenced by coal properties. Majority of the existing
coke quality correlations are based on conventional coal petrogra-
phy including coal rank, relative proportion of macerals and their
⇑ Corresponding author. Tel.: +61 2 93854433.
E-mail address: sushil@unsw.edu.au (S. Gupta).
which is based on the Russian approach [5]. This model considers
all vitrinite, all liptinite and one-third of semifusinite as the reactive
coal matter while the remaining inertinites as well as the mineral
matter are treated as the non-reactive component for predicting
coke stability. Reactive macerals are further subdivided into vitri-
noid type or V-type such that an optimum ratio of reactive to inert
components in each vitrinoid is desired to achieve maximum coke
strength [6,7]. This approach predicts ASTM stability factor by com-
bining composition balance index (CBI) and strength index (SI),
where CBI was defined as the ratio of the inert components in coal
to the optimum ratio of reactive to inert components of a coal for a
given rank, while the SI is evaluated to determine the relative coke
strength depending on coal rank and types [6,7]. The same approach
was modified by Nippon Steel to predict cold coke strength [7].
These relationships have been summarized in a past study [8]. Gen-
erally, these correlations are suitable for predicting coke strength of
Northern hemisphere coals but less reliable for Australian coals
which often contains higher proportion of reactive inertinites
[9,10]. Particularly, the consideration of one-third of total semifusi-
nite as the reactive proportion of relatively lower rank coals (Ro, max
<1.35) is not suitable for many Australian coals.
A coal reflectogram provides the reflectance distribution of coal
sample in the form of a frequency histogram. Random or maximum
vitrinite reflectance of the coal is measured following standard
techniques and the results are usually reported at a fixed interval

0016-2361/$ - see front matter Ó 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.fuel.2011.09.045
 S. Gupta et al. / Fuel 94 (2012) 368–373 369

of 0.05% reflectance (half V-step or V-type). Random vitrinite 2. Experimental

reflectance is measured under non-polarized light, the reflections
from all directions on the vitrinite surface are integrated to give
a mean vitrinite random reflectance (Rr) percent [11]. Maximum
vitrinite reflectance is measured in polarized light whilst the
microscope stage is rotated through 360°. Automatic microscopy
provides mean random vitrinite reflectance data which can be con-
veniently related to consistently higher values of mean maximum
vitrinite reflectance (Rv, max or Ro, max). Current practice of the
measurement of vitrinite reflectance is subjective, time-consuming
and invariably requires skilled petrographer, and hence often leads
to large variance in the measurements [12,13]. Therefore, auto-
matic microscopy of coals is increasingly preferred over manual
point count approach [11–18]. A limited number of studies have
used automated microscopic approach to characterize coke mi-
cro-textures [18–21] and relate to coal rank [18] or blast furnace
coke properties including coke strength [21].
With increasing advances of coal imaging techniques, it seems
feasible to address some of the concerns towards developing an
objective and universal approach for characterizing coal composi-
tion [4,11–18]. On the basis of semi-automated coal reflectance
data, the rank (vitrinite reflectance) and type (maceral group
abundance) of coal was combined to provide a single parameter
i.e. Full Maceral Reflectance (FMR), which could be related to coal
and coke properties [14]. The FMR has been a comprehensive
parameter as it considers the reflectance of all grains including
that of inertinites whose reactivity is known to be rank dependent.
The main aim of this study is to investigate the suitability, limita-
tion and scope for further improvement of that automated micro-
scopic approach in predicting coke strength. Therefore, the FMR
parameter was obtained for a wide range of coals from around
the globe and related to coke strength, reactivity and micro-tex-
ture data. The FMR parameter was modified to develop a new coal
quality index which considered the reflectance contribution of all
maceral groups and the contribution of inorganic matter of coal.
The combined coal index is shown to improve the coke strength
prediction.
2.1. Sample selection
Seven Australian, two Canadian, one Chinese and one Russian
coals were selected on the basis of rank variation. Proximate, ulti-
mate analysis and oxide analysis of the coals is provided in Table 1.
2.2. Semi-automated reflectance measurements
Semi-automatic full maceral reflectogram (FMR) of each coal
was measured at CSIRO, Brisbane. Coals crushed with in a size
range from 212 lm or 90 lm were used to produce grain
mount samples with a packing density of about 30% coal and
70% mounting resin for microscopic analysis. In order to avoid pos-
sible artifacts associated with subsurface particles, a soft polyester
resin containing a special red dye was used to prepare the grain
mount samples. After curing, the blocks were cut perpendicular
to the settling plane. After polishing, the cut surface was used as
specimen for acquiring reflectance data. Full phase reflectograms
were automatically produced for each coal using an 8-bit CCD cam-
era attached to a Carl Zeiss Axiophot microscope. The imaging sys-
tem was setup to provide monochromatic illumination at 546 nm
(green light) and calibrated for intensity using reflectance stan-
dards. Each digital image represented an area of approximately
268  256 lm2 and had a resolution of 512  512 pixels and 256
gray levels. Each pixel represented approximately 0.25 lm2 of
the original coal surface and each image covered up to
65,536 lm2. The field of view covered by an image was much lar-
ger compared to the spot area (up to 25 lm2) often used in case of
manual point count analysis as detailed elsewhere [14,15]. Fig. 1
illustrates typical reflectance curve of a coal sample. An experi-
mentally determined correlation between mineral abundance
and ash value can be used to determine the dark mineral compo-
nent of the reflectogram, which gives the FMR information for
the maceral constituents. However, present paper aims to use

Table 1
Proximate, ultimate and oxide analysis of coals.

Coal samples
AC1 AC2 AC3 AC4 AC5 AC6 AC7 CA1 CA2 CC1 RC1
Proximate analysis (db%)
Moisture % 0.57 0.63 0.90 0.57 0.81 0.95 0.75 0.64 0.93 0.72 0.52
Ash yield % 10.26 9.55 9.19 11.90 6.74 9.87 9.68 8.34 9.45 10.97 9.10
Volatile % 16.70 20.17 22.82 25.31 31.58 31.70 35.56 17.58 23.15 25.79 18.01
Fixed carbon 72.46 69.64 67.08 62.22 60.87 57.47 54.01 73.44 66.47 62.52 72.37
Ultimate analysis (db%)
Carbon % 91.09 91.77 90.38 89.00 87.39 84.46 85.55 93.40 91.31 89.00 93.49
Hydrogen % 4.90 5.04 5.37 5.09 5.69 5.52 6.01 4.73 5.12 5.31 4.82
Nitrogen % 2.01 2.05 2.25 2.00 2.26 1.90 2.19 0.98 1.26 1.55 0.75
Sulfur % 0.65 0.60 0.54 0.53 0.64 0.52 0.53 0.50 0.46 1.21 0.22
Oxygen % 1.36 0.54 1.46 3.38 4.02 7.60 5.72 0.39 1.85 2.94 0.72
Oxide analysis (wt.%)
SiO2 57.5 69.9 54.4 53.4 52.6 72.0 50.2 60.4 59.1 45.8 45.8
Al2O3 30.3 23.3 32.1 25.6 37.6 19.2 28.7 26.5 30.0 39.2 33.1
TiO2 1.6 1.3 1.5 1.3 1.9 1.0 1.5 1.3 1.6 1.8 1.4
Fe2O3 5.7 2.2 4.6 8.5 3.4 4.1 5.7 2.5 2.7 4.3 6.0
CaO 1.6 0.9 2.1 4.4 1.5 0.9 5.6 3.6 2.7 3.6 5.7
MgO 0.6 0.4 0.7 1.0 0.4 0.6 1.8 0.4 0.4 0.9 1.8
K2O 1.0 0.9 1.3 1.4 0.9 1.0 1.1 0.8 0.8 0.4 0.6
Na2O 0.3 0.4 1.3 0.5 0.5 0.4 1.1 0.7 0.1 0.2 0.4
SO3 0.6 0.3 0.3 2.6 0.2 0.7 3.9 2.0 0.7 3.1 4.7
P2O5 0.8 0.4 1.6 1.3 0.9 0.1 0.4 1.7 1.9 0.8 0.5
SiO2/Al2O3 1.90 3.00 1.70 2.09 1.40 3.75 1.75 2.28 1.97 1.17 1.38
MBIa 1.29 0.62 1.38 3.18 0.73 1.11 2.90 0.94 0.93 1.63 2.04
a
Mineral Basicity Index (MBI) = 100 * ash content (%) * (Fe2O3 + CaO + MgO + K2O + Na2O)/((100  VM (%)) * (SiO2 + Al2O3)).
370 S. Gupta et al. / Fuel 94 (2012) 368–373

CMSI ¼ ða þ 2b þ 3c þ 4d þ 5eÞ=ða þ b þ c þ d þ eÞ ð1Þ

In this equation a, b, c, d and e represent percentage of very fine,
fine, medium, coarse and elongate domains respectively.

3. Results and discussion

Vitrinite maceral abundance was obtained from the semi-auto-

Fig. 1. Typical semi-automated curve plotting cumulative frequency against
reflectance.
reflectance values directly therefore dark minerals and liptinite
were not distinguished. Coal maceral and the FMR values based
on the reflectance measurements are provided in Table 2.
2.3. Coke sample preparation
mated reflectance data as detailed elsewhere [14]. Fig. 2 shows that
vitrinite percentage of coals based on the semi-automated micro-
scopic is generally lower than the percentage of vitrinite based on
manual point count data. The differences of vitrinite estimates seem
to be higher for lower rank coals particularly for those with Ro value
less than 1%. Manual vitrinite estimates of coals CA2 and AC7 is sig-
nificantly higher compared to the automated estimates. Comparison
of point count data from three laboratories showed up to 5% stan-
dard deviation of vitrinite estimates [22]. This difference can be
attributed to the sample preparation, maceral identification stan-
dards and the subjectivity of operators. In this paper, all further anal-
ysis is based on semi-automated reflectance data.

Coke samples were prepared under similar conditions in a 30 kg
moveable wall test coke oven facility at Pohang at a fixed heating
rate. The test coke oven length, height and width are 400 mm,
600 mm, 220 mm respectively. In order to achieve better simulation
of industrial operation, the oven is equipped with two doors and one
charge hole on the top such that charging density is about 730 kg/
m3. The wooden boxes were used to fix charging amount of coal. Fi-
nal coking temperature was set to 1373 K and the oven was electri-
cally heated at the rate of 3° per minute for 7 h before pushing cokes.
Cokes were quenched in a box with nitrogen. Coke strength data
including DI150
15 (referred as DI in this paper) and the CRI/CSR were
also measured at POSCO laboratories. Coke strength data is given
in Table 3.
2.4. Coke micro-texture
Table 4 provides coke texture data. Isotropic and non-isotropic
textures were examined using point count analysis at ALS Labora-
tories, Brisbane following Australian convention [19]. Table 4 also
includes Coke Mosaic Size Index (CMSI) based on different mosaic
types using:
3.1. Full Phase Maceral Reflectance Parameter (FMR)
A coal parameter based on semi-automated reflectance can be
calculated from the full phase reflectance data as detailed
elsewhere [14]. Accordingly, each of the 256 reflectance value
was multiplied by the frequency of the associated coal grains and
then combined to provide a single number to incorporate the con-
tribution of individual coal grains [14]. The ‘‘FMR’’ parameter,
which includes the rank (vitrinite reflectance) as well as the type
(maceral group abundance), is the characteristics of whole coal
sample. This is an objective composition parameter and incorpo-
rates the reflectance contribution from each coal grain examined.
This eliminates the subjective identification of maceral group.
The calculated FMR value of all coals is given in Table 2.
Fig. 3 shows that the mean maximum vitrinite reflectance (Ro,
max) of coal samples based on automated microscopic data in-
creases with increasing FMR parameter. The Ro, max values of
the coals also indicated a good correlation with the same based
on the manual point count data from the POSCO laboratories not
shown in this paper. This shows that automated reflectance data
can reliably assess the coal rank values.

Table 2
Coal macerals and FMR values based on semi-automated reflectance measurements.

Coal samples
AC1 AC2 AC3 AC4 AC5 AC6 AC7 CA1 CA2 CC1 RC1
Vitrinite % 72.6 68.1 77.4 45.1 68.3 65.5 68.7 55.6 47.5 59.3 80.1
Inertinite % 17.5 25.4 16.9 45.9 23.1 17.5 12.8 35.2 44.5 32.7 10.2
Liptinite % 9.5a 6.2a 0.5 3.8 3.4 11.8 13.3 9.0a 2.8 2.8 9.6a
Dark mineral % 4.9 5.0 4.9 5.0 5.0 5.1 4.7
Bright mineral % 0.4 0.2 0.3 0.2 0.3 0.2 0.2 0.2 0.1 0.5 0.2
Rr 1.57 1.30 1.15 0.91 0.82 0.67 0.64 1.47 1.04 1.07 1.60
Ro, max 1.67 1.38 1.22 0.96 0.87 0.71 0.68 1.56 1.11 1.13 1.71
FMR 165 144 124 124 97 78 69 167 127 136 161

Rr and Ro, max indicate mean random and mean maximum vitrinite reflectance percentage.
a
Sum of Liptinite and dark minerals.

Table 3
Coke strength data.

Coke samples
AC1 AC2 AC3 AC4 AC5 AC6 AC7 CA1 CA2 CC1 RC1
 
DI or DI150 79.3 80.9 81.8 72.6 79.1 74.1 69.7 67.8 80.8 81.4 81.8
15

CSR 71.7 73.2 68.5 30.9 55.2 21.5 17.8 63.4 69.7 57.9 38.3

Data based on measurement at POSCO laboratories [22].

 S. Gupta et al. / Fuel 94 (2012) 368–373 371

Table 4
Micro-texture data of cokes.

Coke samples
AC1 AC2 AC3 AC4 AC5 AC6 AC7 CA1 CA2 CC1 RC1
Organic inclusion
Isotropic porous % 10.9 12.0 8.9 16.8 6.2 53.6 11.9 9.7 18.2 10.8 8.4
Iso. non-porous % 0.4 1.8 1.2 6.6 2.0 1.0 0.2 1.0 1.0 1.8 1.2
Fused carbon domain
Very Fine – – – 6.2 71.3 29.8 72.9 1.4 5.6 6.8 0.8
Fine – – 1.8 60.2 17.0 9.3 8.1 1.0 25.3 48.2 0.8
Medium – 7.8 77.8 5.0 0.2 1.2 1.0 6.3 47.7 19.7 4.2
Coarse 7.9 74.5 7.7 – – – – 19.6 0.6 9.8 56.5
Elongate 76.8 1.2 – – – – – 56.9 – 0.4 25.9
CMSI 4.91 3.92 3.07 1.98 1.20 1.29 1.12 4.52 2.55 2.40 4.20
Mineral matter 4.0 2.8 2.6 5.2 3.2 5.2 5.9 4.0 1.6 2.6 2.2

Note: Data is based on measurements at ALS laboratories. AC5 contained 0.2% pyrolitic carbon also.

Fig. 2. Comparison of coal vitrinite estimates based on semi-automated microscopic and manual point count data. The calculated Ro, max values based on semi-automated
data are also indicated.

Fig. 3. Correlation between Ro, max and FMR and (b) correlation between calculated Ro, max values based on the CSIRO semi-automated measurements and POSCO manual
petrographic data.

The FMR parameter directly correlates with total carbon con-
tent (Fig. 4a) and inversely with volatile matter of coals (Fig. 4b).
High FMR value is generally indicative of high ordering of carbon
structure (Fig. 4c). Total vitrinite content of coals did not show
any correlation with FMR values.
The FMR values of the tested coals were high for low fluidity coals
but did not show any clear correlation with maximum Gieseler
fluidity values (Fig. 5). The FMR parameter did not indicate any
satisfactory correlation with carbonization parameters such as total
dilation, free swelling index and Gieseler maximum fluidity data.
3.2. Association of FMR and coke properties
The FMR parameter did not provide any correlation with fusible
carbon content of cokes. However, coal FMR parameter indicated a
good correlation with coke mosaic size index (Fig. 6) such that high
FMR coal resulted in large CMSI of the tested samples.
Fig. 7a shows the correlation between coal FMR and cold coke
strength (DI150
15 or DI). The DI values of cokes increase with increasing
coal FMR values with the exception of AC4 and CA1 samples. The
same figure further illustrates that consideration of only Australian
coals (shown as solid circles) improves the correlation with the
exception of AC4 sample. This study suggests that medium FMR
range (100–150) of coals leads to high cold strength (DI > 80). The
FMR parameter indicated a similar trend with CSR values of cokes
(Fig. 7b). High FMR coals were generally associated with high CSR
values of cokes indicating a better correlation for Australian coals.
Coal AC4 is relatively lower rank while both CA1 and AC4 are
rich in inertinite such that their inertinite to vitrinite ratio is great-
er than 0.6. Both rank and inertinite could contribute to lower DI
372 S. Gupta et al. / Fuel 94 (2012) 368–373
Fig. 4. FMR parameter vs. carbon content (a), volatile matter (b), and Lc (c) values of coals.
Fig. 5. Maximum fluidity of coal vs. FMR parameter.
Fig. 6. Coal FMR parameter vs. Coke Mosaic Size Index (CMSI).
and CSR values. The FMR values of both coals are much higher
compared to the FMR values of other coals of adjacent ranks (Table
2). The exact reason for the higher FMR values of these coals is not
clear as in addition to high amounts of inertinite, differences in
rank and mineral types particularly pyrite could also influence
the reflectance data of coal grains and hence the FMR values.
Therefore, further efforts will focus on clarifying the exact reasons
of high FMR values of certain coals and their association with mea-
sured coke strength.
3.3. Combined coal index and coke strength
The FMR parameter was modified by tuning the possible contri-
bution of inertinite and inorganic matter on FMR parameter. Coal
reflectance data was further processed by using a number of itera-
tions such that the reflectance contribution of coal grains in the
gray-scale range of 12–62 was decreased to 0.95 and those in the
gray-scale range of 91–118 was decreased to 0.6 times of that ori-
ginal values. On the basis of known influence of coal mineralogy on
coke strength at high temperatures [23], a small correction for
inorganic matter can also be introduced in the FMR parameter. In
past, effect of ash chemistry on the CSR was related through Min-
eral Basicity Index [13]. The impact of inorganic matter of coals
was incorporated into the above corrected FMR parameter by
dividing with the square root of Mineral Basicity Index (MBI). By
combining two types of modifications in the original FMR param-
eter as discussed above, a new parameter is proposed which is re-
ferred as combined coal index (CCI).
Fig. 8a and b correlate CCI with cold coke strength (DI) and CSR
respectively. These figures clearly illustrate that the new coal index
improved the correlations with both cold and hot strength of coke
after reaction except for coal CA1. These Figures shows that as the
CCI values exceed 80, DI and CSR exceed more than 80 and 60
respectively except coal CA1. It seems the DI value of Canadian coal
CA1 unexpectedly low but exact reason is not clear. Fig. 8 further
shows that the correlation is better in case of Australian coals only.
Therefore, under similar coking conditions, high CCI coals are ex-
pected to provide cokes of high cold and hot strength after reac-
tion. This new parameter completely eliminates the need of
subjective identification of coal maceral or sub-maceral groups, it
still requires validation for a larger set by coals of varying inertinite
and mineralogy. The proposed parameter is expected to be applica-
ble to coal blends but would require some additional processing
and validation. Subsequent publications will consider the implica-
tions of coal blending particularly relating to consequences of
differences in geological origins.
 S. Gupta et al. / Fuel 94 (2012) 368–373
Fig. 7. (a) DI vs. FMR and (b) CSR vs. FMR. Australian samples are shown as solid circles.
Fig. 8. (a) Correlation between CCI and DI and (b) CCI and CSR. Australian cokes are shown as solid circles.
4. Conclusions
A wide range of coals were used to establish a correlation be-
tween coal reflectance and coke strength. Coals were characterized
using automated optical microscopy. Coal petrographic results
based on automated microscopy were generally found to be con-
sistent with the manual point count data. The FMR parameter
based on reflectance of individual coal grains showed satisfactory
correlations with coal rank, total carbon content and volatile mat-
ter. The FMR parameter was modified to dilute the contribution of
high reflectance coal grains as well as oxide ash chemistry of coals
to propose a new combined coal index (CCI). The new index is
shown to provide better correlation with both cold and hot coke
strength after reaction. The new coal index eliminates the reliance
on subjective and manual identification of macerals and is applica-
ble to a wider range of coals. The proposed combined coal index
provides a promising objective measurement based alternative
for predicting coke strength. The proposed index can be further im-
proved by considering the differences in the nature of inertinite
and mineralogy of similar rank coals from different geological
origins.
Acknowledgements
We acknowledge the financial support provided by POSCO for
this study and also the permission to publish this work. Authors
also appreciate the help provided by Karryn Warren from CSIRO
for coal analysis.
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