Coal characterisation by automated coal petrography

q
G. OBrien
a,
*
, B. Jenkins
b
, J. Esterle
a
, H. Beath
a
a
Queensland Centre for Advanced Technology (QCAT), CSIRO Exploration and Mining, P.O. Box 883, Kenmore, Brisbane, Qld 4069, Australia
b
Queensland Centre for Advanced Technology (QCAT), Jenkins Kwan Technology Pty Limited, Brisbane, Qld, Australia
Received 9 July 2002; revised 9 July 2002; accepted 19 December 2002; available online 17 January 2003
Abstract
Automated imaging techniques were rened to characterise the rank and maceral composition of coals by a full maceral reectogram of
polished coal grain mounts. Precision was improved by processing individual grains in each image separately and correcting within the
software for the topography that occurs between the different macerals and minerals in the grains. Maceral group proportions and vitrinite
reectance information extracted from these reectograms compared well with manual results for a comprehensive suite of Australian coals
varying in rank from a mean vitrinite reectance of 0.482.13%. A parameter that combines rank and type calculated from the reectograms
correlated strongly with chemical properties determined by ultimate and proximate analyses. For a limited number of samples, for which
coking tests had been performed, this parameter also correlated with estimated coking performance.
Crown Copyright q 2003 Published by Elsevier Science Ltd. All rights reserved.
Keywords: Full maceral reectogram; Coke strength after reaction; Coke reactivity index; Image calibration; Topography correction
1. Introduction
Coal petrography is a standard method for characterising
the organic (maceral) and inorganic (mineral) constituents
of coal. Two types of data are derived from this method:
rank (dened by vitrinite reectance) and composition
(maceral proportions). Petrographic analyses are used by
geologists to gain an understanding of coal deposition, by
coal technologists to evaluate coals for coking potential, and
by coal quality personnel to monitor the quality of mine
product or shipment coal. These analyses also provide a
powerful forensic tool for monitoring coal blending and for
detecting and identifying contamination. Coal petrography
has also been used since the 1950s to predict coking
performance [1]. The established model was developed for
vitrinite-rich North American coking coals to predict ASTM
coke stability values [2], but in recent times coke strength
after reaction (CSR) and coke reactivity index (CRI) have
assumed a more important role for rating the marketability
of coals internationally. It was shown that the ASTM coke
stability predictions did not apply correctly to coals that
contained signicant proportions of highly reactive inerti-
nites [3]. This study also showed that inertinite reactivity
was related to reectance and concluded that inertinite
reactivity was rank dependent. These ndings suggest that
the full maceral reectogram (FMR) may be used for
improved coke stability predictions of coals with signicant
amounts of reactive inertinite, and could potentially be used
to predict CSR and CRI.
In order to reduce operator subjectivity and improve the
accuracy of petrographic analyses, there have been a
number of projects that have used image analysis to
automate the process [411]. Since these earliest of these
projects were conducted, both camera and computing
equipment have improved. Earlier charge-coupled device
(CCD) cameras detected 64 grey scales (6-bit) whereas
more modern ones detect from 256 grey scales (8-bit) to
16,384 grey scales (14-bit). An increase in personal
computer memory size and speed by several orders of
magnitude have made it possible to apply the most complex
image processing algorithms to the problem. Due to the
essentially colourless nature of coal, the use of grey scale
images has remained the preferred method for coal image
microscopy.
The grey scale of each pixel in a coal image can be
calibrated to provide a measure of the reectance at that
point. Hence, a reectance distribution of all maceral and
mineral species plus the mounting resin can be obtained
from a sample of images. Once regions containing mounting
0016-2361/03/$ - see front matter Crown Copyright q 2003 Published by Elsevier Science Ltd. All rights reserved.
doi:10.1016/S0016-2361(02)00428-3
Fuel 82 (2003) 10671073
www.fuelrst.com
q
Published rst on the web via Fuelrst.comhttp://www.fuelrst.com
*
Corresponding author. Tel.: 61-7-3327-4457; fax: 61-7-3327-4455.
E-mail address: graham.obrien@csiro.au (G. OBrien).
resin are removed from the images, the remaining areas
contain the maceral reectance distribution of the coal
maceral and mineral entities. A FMR is a ngerprint, which
can be represented as the cumulative frequency of all
maceral and mineral entities plotted on a probability scale
against reectance. The vitrinite reectance values display a
normal distribution, and plot as a straight line on this
probability scale [10] and hence within the FMR, inection
points coinciding with the commencement and end of the
vitrinite proportion can be used to determine maceral group
proportions (Fig. 1). For single seam coals, the midpoint of
the vitrinite population when plotted this way is a method of
dening the rank of the coal (mean vitrinite reectance). In
single coals, the maceral groups have discrete reectance
ranges, with little overlap. The liptinite group and most
minerals are lower in reectance than vitrinite, whereas the
inertinites are higher. Some minerals, such as iron suldes
and oxides are higher again.
2. Methods
Test work was carried out at the Queensland Centre for
Advanced Technology (QCAT) in Brisbane, Australia.
Analyses were carried out in two steps. In the rst step,
maceral proportions and random vitrinite reectance were
determined to Australian Standards [12,13], and FMRs were
determined manually using a Carl Zeiss Axioplan micro-
scope. In the second step, full phase reectograms were
automatically produced for each coal using an 8-bit CCD
camera attached to a Carl Zeiss Axiophot microscope that
was linked to an image analysis system.
2.1. Sample preparation
Sample preparation to Australian Standard [14]
was found to produce imaging artefacts under some
circumstances. A new method was developed that used a
soft acrylic resin containing a special red dye [15]. The
acrylic resin was chosen because of its similar hardness to
coal, which minimised the polishing relief of the coal
particles. The red dye was chosen for its ltering effect of
the green incident light. This helped to delineate coal
particle edges and to reduce diffuse reections from
particles below the resin surface.
Some of the coals had been prepared with a 1 mm top
size and others were ner (2212 mm or 290 mm) with a
packing density of about 30%. After curing, the blocks were
cut perpendicular to the settling plane and the cut surface
was polished to produce a relief free surface.
2.2. Image collection and processing
The imaging system was setup to provide monochro-
matic illumination at 546 nm (green light) and calibrated
for intensity using reectance standards. Each digital
image represented an area of approximately
268 256 mm
2
and had a resolution of 512 512 pixels
and 256 grey levels. Hence each pixel represented
approximately 0.25 mm
2
of the original coal surface and
each image covered up to 65,536 mm
2
. The eld of view
covered by an image was much larger than the spot area
(up to 25 mm
2
) used in a standard manual analysis. This
meant an image contained signicantly more variability in
illumination and glare. A microscope optimized for
uniform illumination normally has a 1020% variation
in incident light across the eld-of-view. Therefore, a
calibration procedure was used to map the incident light
intensity at each pixel position. These incident light maps
were produced for several calibration standards of
differing reectance prior to each coal specimen being
imaged. These maps were stored and used later in the coal
image processing stage. The number of coal images
Fig. 1. FMR of a single seam coal.
G. OBrien et al. / Fuel 82 (2003) 10671073 1068
acquired depended on the size fraction of the coal sample
and sampling accuracy required.
The image processing routine commenced with the
input of the sample management details. This included
details about size fraction and coal type, which affected
the image processing method. The rst step involved
resin identication. The method was based on reectance
and morphology differences. The added complexity of
using morphological parameters was due to a lack
of reectance uniqueness between resin and some types
of dark minerals, liptinites and pores. Once the mounting
resin was removed from the image, the coal grains were
processed individually. This improved the accuracy of
artefact removal (such as scratches, and topography).
Scratches were removed during image processing by
assigning the affected regions the reectance of contiguous
macerals. Polishing topography caused by the differences in
hardness between sample constituents was removed next.
Topography causes incident light to be scattered and can
reduce the measured reectance values. In manual petro-
graphy, operators avoid such areas and select the attest
parts within a maceral for reectance measurements.
However, an imaging system cannot avoid areas affected
by topography.
Fig. 2 shows part of a grain that has been appreciably
enlarged so that the image shows the classic blocky pixel
pattern and the effects of topography. In the image, the areas
surrounding bright minerals and inertinite macerals can be
black whereas the inertinite itself can have variable grey
scale values due to topography. The vitrinite can also have
topographic features as it tends to be eroded preferentially to
the mounting resin and neighbouring harder macerals. A
typical coal particle therefore consists of vitrinite with
negative polishing relief whereas the inertinites show
positive relief.
Fig. 3 demonstrates the effects of the main image
processing stages on producing a calibrated coal reectance
distribution. The introduction of topography correction
improved the separation between maceral populations,
increased inertinite reectance and abundance, and lowered
mineral matter content.
For the single seam coking coals, some 30 million
individual readings, from at least 500 grains (200 images),
were measured for each sample. For a typical 290 mm
pulverized coal, the analysis used at least 5000 grains in
about 100 images.
Fig. 2. Part of an image that has been appreciably enlarged to show the
effects of polishing induced topography.
Fig. 3. Coal reectance distributions for unprocessed (raw) images, illumination corrections, without topography correction, and with topography correction.
G. OBrien et al. / Fuel 82 (2003) 10671073 1069
2.3. Data analysis
The output from the image analyser consists of counts
recorded at each grey scale and data obtained from the
reectance standards. This output initially was processed in
Microsoft Excele. An automated macro program:
converted grey scale values into reectance values;
constructed the reectogram; and
determined the inection points and maceral group
proportions.
In addition, each of the 256 reectance values was
multiplied by its frequency of measurements and then
summed to provide a single number to describe the
reectogram. This number was termed the FMR parameter.
This is inuenced by the rank (vitrinite reectance) and type
(maceral group abundance) of the coal and provided a
simple index for representing the coals petrographic
composition.
3. Results
3.1. Image output
To date, approximately 40 coals of various ranks have
been analysed. A FMR for a low rank thermal coal (Fig. 4),
a single seam coking coal (Fig. 5) and a semi anthracite
(Fig. 6) demonstrate that the technique is applicable to
coals from a wide rank range. The thermal coal shown in
Fig. 4 and the semi anthracite shown in Fig. 6 are the
lowest and highest rank coals that have been analysed to
date.
The maceral abundance results from manual and
automated methods are given in Fig. 7. Maceral group
proportions estimated from the FMR using data without
topography correction agreed well with manual results for
vitrinite abundance but slightly underestimated inertinite
proportion and overestimated liptinite plus minerals.
Incorporation of topography correction into image proces-
sing decreased the abundance of low reecting material and
Fig. 4. FMR for a low rank thermal coal (5000 grains in 100 images were analysed).
Fig. 5. FMR of a single seam coking coal (596 grains in 200 images were analysed).
G. OBrien et al. / Fuel 82 (2003) 10671073 1070
increased inertinite abundance while leaving vitrinite
abundance essentially unchanged.
The automated coal petrography system was found to be
excellent for determining mean random vitrinite
reectance (Rr) for the entire range of coals studied to
date. The correlation with manual results (Fig. 8) was
essentially 1-to-1 with an R
2
of 0.995.
4. Discussion
4.1. Current rank limits
The lowest rank coal successfully analysed had a mean
random vitrinite reectance of 0.48%. Analysis of coals of
lower rank would require the sample preparation and image
collection method to be further rened, but there has not
been a commercial incentive to pursue this. The highest
rank coal successfully analysed to date had a mean random
vitrinite reectance of 2.13%.
4.2. Relationships between FMR and coal properties
The FMR parameter is a simple method for combining
coal rank and type information. For two coals with the same
composition, the one with greater rank will have the greater
FMR parameter value and similarly for two coals with the
same rank, the one with the greater inertinite proportion will
have the greater parameter value. The FMR parameter
correlated well with the bulk coal properties of volatile
matter (Fig. 9), carbon content (Fig. 10), and hydrogen
content (Fig. 11). Whereas, carbon content correlated
equally well with vitrinite reectance, volatile matter and
hydrogen content displayed signicantly better correlations
with the FMR parameter than with vitrinite reectance, due
to their sensitivity to type [16]. One coal (identied in
Fig. 11 as an anomalous value) had signicantly low
hydrogen content and did not t the basic characteristics of
the other coals.
The FMR parameter showed promising correlations with
coking performance, as measured by CRI (Fig. 12) and CSR
(Fig. 13) for the small number (six) of coals for which
coking tests had been performed. With increasing FMR
Fig. 6. FMR of a semi anthracite (580 grains in 200 images were analysed).
Fig. 8. Relationship between Rr determined from manual analysis and the
automated coal petrography system.
Fig. 7. Maceral group abundances obtained from manual analysis and the
automatic coal petrography system.
G. OBrien et al. / Fuel 82 (2003) 10671073 1071
parameter, CRI decreased and CSR increased. The range of
FMR parameter values that can be correlated with coking
performance are yet to be determined. It is expected that,
there will be minimum and maximum parameter values
coinciding with the commencement and end of the coking
range.
4.3. Maceral subgroups
In manual coal petrography, the classication of
macerals also takes place at the maceral subgroup and
maceral level. For example, an analysis subdivides
the vitrinite group into the subgroups telovitrinite,
detrovitrinite and gelovitrinite [12]. Reectance alone
cannot provide sufcient information for subdividing the
vitrinite group into subgroups and requires integration
with texture and fabric. The reectogram provides the
proportions of high and low reecting inertinites, but
without size and maceral association, it cannot dis-
tinguish inertodetrinite and macrinite from semi fusinite
and fusinite. Similar to previous imaging systems,
discrimination of liptinite from dark minerals was
difcult especially for low rank coals.
5. Conclusions and future work
For single seam coals between about 0.4 and 2.1% mean
random vitrinite reectance, an imaging method was used to
produce FMRs and determine mean vitrinite reectance and
maceral group abundances. Good results were obtained
using 8-bit digital technology primarily because of the
improvements made to sample preparation, image cali-
bration, and image processing. Two key developments of
this work have been to process individual grains separately,
and to correct for topography within grains. Additionally,
Fig. 9. Volatile matter content versus FMR parameter.
Fig. 11. Hydrogen content versus FMR parameter.
Fig. 12. CRI versus FMR parameter.
Fig. 13. CSR versus FMR parameter.
Fig. 10. Carbon content versus FMR parameter.
G. OBrien et al. / Fuel 82 (2003) 10671073 1072
the reectance information collected on all maceral and
mineral species correlated with bulk chemical properties
and coking performance. Further tests are required to
explore the relationships between coal properties and the
FMR parameter for coal blends and unusual coals (e.g.
those having suppressed vitrinite reectance). It is hoped
that this will lead to a technique that can provide a better
understanding of coal maturation history and antagonistic
and synergistic effects in coal blends.
The system produced calibrated images of individual
grains. These images will provide a basis for future studies
of maceral texture and associations and development of a
maceral subgroup analysis method, and a blend analysis
method.
Acknowledgements
The authors thank the Australian Coal Association
Research Program (ACARP) for their nancial support of
this work. BHP Billiton Mitsubishi Alliance Coal has
provided samples and valuable technical discussion. The
assistance of G. Corrin is gratefully acknowledged.
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