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Table 1. Generalized Stratigraphic Succession of the Raniganj Coalfield33 (Modified After GSI, 2003)
and associated matrix pores and their influence on coal similar process that creates jointing in other rocks. The strike
physicomechanical properties. directions of cleats can be related to folds12 and thrust fault13
Some authors have categorized the origin of cleats in coal beds although local and lateral disturbances occur because of
as endogenetic, where development is related to compaction, differential compaction and load release; erosion complicates
dehydration, and devolatilization during coalification, and some
the coal cleat system. Nickelsen and Hough14 suggested that face
others as exogenetic, where cleat formation is thought to result
from basin tectonic forces.2,4,5,11 When coal reaches the high- cleats are formed as extension fractures parallel to the direction
volatile bituminous stage and physical properties have reached a of maximum, horizontal crustal shortening at the time of folding.
state prone to fracturing, changes in tectonic forces fracture the Stone et al.15 found that the butt cleat system in the Powder
coals. Tectonic forces control the formation of coal cleats in a River basin coal seam is nearly parallel to the structural flexures
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Figure 1. Geological map of Raniganj Coalfield showing coal core sampling locations31−36 (after Gee, 1932; Ghosh, 2002; GSI, 2003; Mendhe et al.,
2017, 2018; Mishra et al., 2018).
and fold axis. In contrast, the face cleat system is approximately than other lithotypes27,28 and is very permeable due to its good
perpendicular to the basin axis. connectivity between pores and cleats. However, clarain has
Alstine and Butterworth13 supported the theory of cleat moderate permeability, which depends on the content ratio of
formation during and in response to tectonic events. Face cleats vitrinite and durain. The lithotypes durain and fusain are known
are generally found perpendicular to the thrust fault strike and for their low permeability due to the high concentration of clay
the axial trend of local fold hinges, i.e., parallel to the plane of mineral, decomposed material, and inertinite content.29,30
maximum compressive principal stress.12 In contrast, butt cleats In this study, an attempt has been made to investigate the
would have formed during the release of the stress field various coal properties and their contribution to cleat origin,
responsible for the face cleat formation. According to Dawson occurrence, and influence on strength properties. Coal core
and Esterle,11 the cleat spacing in dull coal is wider than in bright samples obtained from eight vertical boreholes from Raniganj
coal, and master cleats extend across vitrain bands. Generally, Coalfield were analyzed for cleat intensity, lithotypes, geo-
macropores are more and micropores are fewer in inertinite-rich chemical constituents, petrographic compositions, X-ray
coals than in vitrinite-rich coals of the same rank.16,18 As the coal diffraction (XRD) spectroscopy for mineralogy, scanning
rank increases, the number of meso- and macropores reduces, electron microscope (SEM) study for microcleat/fractures,
which impacts the matrix strength properties of coals.19 and their physicomechanical properties. Pore distribution and
The lithotype bands in coal that can be megascopically geometry were evaluated by the Brunauer−Emmett−Teller
recognizable by the naked eye have different macerals and (BET) analysis and related to cleat/fracture. Various relation-
consist of complex mixtures of organic matter and minerals.20−22 ships were established to determine the role of maceral,
The variation in the lithotype thickness of coal indicates the geochemical constituents, and inorganic content on cleat
heterogeneous supply of vegetation and sediments in the swamp formation. Also, the strength of coal seams has been discussed
and change in the depositional conditions. Usually, it has been based on cleat intensity and organo−inorganic content. This
observed that the inertinite content increases with the gradual study will understand in depth the coal seam characteristics
decrease in the vitrinite content, attributed to geochemical considering the influence of cleat/fracture on geomechanical
alterations and inertinization of the vitrain lithotype.21,23−25 The strength. It may have broad application in mine planning and
change in chemical properties of lithotypes is due to the design, efficient coal extraction, rock mechanics, roof supports,
difference in maceral compositions, i.e., fusain is typically more coal beneficiation, and methane recovery from coal seam
aromatic than other lithotypes because of the change in the reservoirs.
functional group during coalification from aliphatic to aromatic
compounds. The chemical properties of vitrain, clarain, and 2. STUDY SITE: RANIGANJ COALFIELD
durain lithotypes may vary and be related to the amount of The Raniganj Coalfield covers 1900 km2 occurring in a
liptinite, vitrinite, and inertinite macerals.26 From different semielliptical intracratonic rift basin lying between the latitudes
studies, it has been observed that there is a remarkable difference 23°22′ N and 23°52′ N and longitudes 86°36′ E and 87°30′ E
in porosity characteristics among different lithotypes. Mastalerz (Figure 1).31−36 The basins comprise the Gondwana super-
et al.24 demonstrated that fusains in high-volatile bituminous group, which is laterally variable and reaches a thickness greater
coal have the smallest and vitrains have the largest micropore than 3000 m in the south and northeast segments. The
and mesopore volumes. Vitrain exhibits more fractures (cleats) sediments of the Lower Gondwana (Permian) age embody three
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major Formations: Barakar, Barren Measures, and Raniganj coalfield and gradually thins out in the east. The development of
Formations.32,33 coal seams in the Barakar Formation exhibits a substantial lateral
The rocks of the Barakar Formation outcrop in the northern variation. Gee31 identified seven regional coal seams, which are
part of the Raniganj Coalfield. The Lower portion consists of known as BR-I to BR-VII. In the western part of the Barakar
coarse- to very coarse-grained sandstones and conglomerates Formation, i.e., at Mugma, 15 well-developed coal seams are
and a minor bit of shale with three persistent coal seams. Coarse- recorded; at the Central portion, i.e., at the Chanch Barakar−
grained sandstones are less dominant in the middle part and Kulti−Lalganj area, there are eight seams; and at the eastern
contain three coal seams. Coarse- to very coarse-grained part, i.e., at Churulia−Kasta, only the Churulia Top and Bottom
sandstones and conglomerates and a small portion of shale are seams are present. A generalized sequence of coal horizons and
present in the Upper portion and include three persistent coal their local names in the northwestern, north-central, and
seams. The Barren Measures Formation is known as ironstone, a northeastern parts of the Raniganj Coalfield are presented33 in
monotonous dark-gray to black color silty shale sequence of thin Table 1 (GSI). Lithologs of the boreholes from which coal cores
bands and lenses having minerals like cryptocrystalline clay, were received, illustrating the presence of multiple coal seams in
ironstones, siderite, and goethite. The Raniganj Formation the thick Raniganj, Barakar, and Barren Measures Formations,
contains a series of sandstones, calcareous in nature and finer are shown in Figure 2.
than the Barakar Formation, shale, and several well-developed
coal seams. The lithostratigraphic succession of the Raniganj
Coalfield illustrating the location of subsurface horizon of coal
samples is given in in Table 1.
Figure 3. continued
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Figure 3. (a−f): Lithotype variation and nature of banding observed in coal core samples.
banded coal (Bb) bears more cleats or fractures than dull banded The core samples’ fractured surfaces are mostly subconchoidal
coal (Db) and banded coal (Bd) due to brittle characteristics of to even with alternate thick and thin bands of bright and dull.
vitrain. The mixed alternate bands of bright and dull originated They are deposited in a low-energy fluvio-lacustrine freshwater
from coalfield plant fragments and detrital plant material. The reducing condition controlled by river currents and a load of
dull band (Db) developed from partially altered detrital plant sediments.43,44 It is interpreted that the dominance of carbon-
material, generally indicating freshwater conditions with an rich vitrain bands with a high degree of brightness signifies
increased influx of mineral/clay matter. Megascopically, durain anoxic waters that sheltered the organic matter from initial decay
containing dull bands (Db) is grayish to brownish-black and is and a continuous load of sediments sink the basin to a higher
usually the hardest and most resistant lithotype in the studied temperature.
coal.42 The low intensity of dull coal (D) observed in the dull The lithotype intensity of different classified bands was
banded nature (Db) of the studied coal (0.20−1.60%) indicates counted, considering a length of 10 cm (area 10 × 10 cm2)
the relatively less oxic condition due to early initiation of the (Table 3). The intensity of the lithotype is the cumulative
diagenetic process (Figure 3a−f). The fibrous coal (F) surface area of a particular band per unit volume. The
comprising fusain with a silky luster is recorded in traces or dominance of bright (B) and bright banded (Bb) lithotypes
negligible amounts along the bedding planes. The low intensity demonstrates that the environment of deposition was favorable
of other lithotypes like shaly coal (Sc), coal shale (Cs), for organic matter preservation before attaining early anoxic
carbonaceous shale (Cbs), and shale (S) is in the studied coal, conditions. The ternary facies of lithotypes B + Bb, Bd + Db + D
demonstrating significant inputs of organic matter in the basin. + F, and Sc + Cs + Cbs + S are given in Figure 4, specifying the
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Table 3. Lithotype Intensity (%) Counted for Each Coal Core Sample (Considering a Length of 10 cm)
sample no. B Bb Bd Db D F Sc Cs Cbs S fracture connectivity
CG-1901 2.2 3.1 1.2 0.5 0.6 - 0.2 0.2 - - good
CG-1902 3.4 2.9 1.4 0.7 0.2 0.1 0.2 0.3 0.2 - excellent
CG-1903 1.8 1.2 0.5 1.0 1.3 0.2 0.4 0.4 0.2 - fair
CG-1904 1.6 1.8 1.2 1.8 0.6 - 0.9 0.6 0.7 0.2 fair
CG-1905 3.1 2.2 0.9 1.3 0.6 0.4 0.3 0.8 0.2 0.2 excellent
CG-1906 0.9 1.6 3.8 2.7 0.4 0.2 0.1 - 0.2 0.1 poor
CG-1907 3.6 2.1 1.8 0.5 0.5 0.4 0.2 0.4 0.2 0.3 excellent
CG-1908 2.1 1.7 2.1 1.8 1.3 - - - - - good
CG-1909 1.6 2.5 2.3 1.6 0.2 - - 0.2 0.2 0.2 fair
CG-1910 1.2 1.9 2.7 2.0 1.3 0.1 0.2 0.2 0.1 0.2 fair
CG-1911 2.4 1.9 4.1 1.2 - - 0.1 0.2 0.1 - good
CG-1912 1.0 1.6 1.6 2.6 0.8 0.4 0.4 0.1 0.2 0.1 poor
CG-1913 3.4 2.1 1.6 1.2 1.0 0.2 0.1 - 0.2 0.2 excellent
CG-1914 2.6 1.4 2.4 1.4 0.4 0.2 0.6 0.2 - - good
CG-1915 3.0 2.0 1.9 1.7 0.9 - 0.2 - 0.1 - good
CG-1916 1.9 1.6 1.2 1.4 1.2 0.2 0.8 0.1 0.4 0.4 fair
CG-1917 2.1 1.4 1.6 0.8 1.5 0.4 1.2 0.4 0.2 0.6 good
CG-1918 1.8 2.8 0.6 2.8 0.6 1.2 0.4 1.0 0.6 0.2 fair
CG-1919 0.6 1.8 0.7 2.7 0.4 1.6 0.2 1.2 0.4 0.4 poor
CG-1920 1.4 2.1 0.9 1.6 1.2 0.6 0.4 0.7 0.2 0.9 fair
CG-1921 2.4 1.8 3.4 1.3 0.2 - 0.5 0.2 0.2 - good
CG-1922 2.4 2.1 2.4 1.4 0.7 0.4 0.2 0.4 - - good
CG-1923 3.2 1.8 0.2 1.9 0.7 0.2 - 0.4 - - excellent
CG-1924 1.4 0.5 1.6 1.5 1.4 0.2 0.4 0.2 0.4 0.6 fair
CG-1925 1.6 1.4 2.4 2.8 1.6 0.4 0.2 0.1 - 0.1 fair
CG-1926 2.1 1.5 3.1 1.3 1.2 0.2 0.4 0.1 1.2 0.3 good
CG-1927 3.4 2.1 2.4 0.4 0.6 0.2 0.7 - 0.1 0.1 excellent
CG-1928 0.8 1.4 4.6 1.8 0.2 0.4 0.1 0.2 - 0.1 poor
CG-1929 0.3 0.4 2.8 2.1 1.4 0.6 0.2 1.2 0.8 0.2 poor
CG-1930 0.4 0.6 1.8 3.9 0.6 0.2 0.7 1.0 0.4 0.1 poor
CG-1931 1.2 0.8 2.6 2.4 0.8 0.2 0.4 0.1 0.3 0.2 fair
maximum 3.60 3.10 4.60 3.90 1.60 1.60 1.20 1.20 1.20 0.90 poor-to-excellent cleat and fractures
minimum 0.30 0.40 0.20 0.40 0.20 0.10 0.10 0.10 0.10 0.10
average 1.96 1.75 1.99 1.68 0.81 0.38 0.38 0.42 0.33 0.27
stdev. 0.94 0.64 1.07 0.80 0.43 0.35 0.27 0.35 0.26 0.21
Figure 5. continued
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Figure 5. (a−v): Type of cleats recorded in vertical and horizontal sections of studied coal core samples.
coal seams of Barakar and Raniganj. According to Kendall and no. CG-1907 and are inclined to the coal core axis (Figure 5f)
Briggs and Laubach et al.,4,46 cleats are vertical and are and indicates their origin after the heating episode of igneous
characteristically oriented perpendicular to the stratification, intrusion. The photograph of the horizontal and vertical sections
even where beds are deformed, which indicates that the cleat of the coal sample with the schematic illustrating the richness of
generation happened earlier than the structural disturbances of cleats that is the property of vitrain. The face and butt cleats are
the beds. partially deformed (Figure 5l). The gelification effects on the
All of the coal samples of the Raniganj Formation, e.g., CG- face, butt, and master cleats caused by thermal transformation
1901 to CG-1904 and then CG-1916 to CG-1931 (Figure 5a−d during the bituminization process are indicated in Figure 5m.
and l−v), show well-developed face and butt cleat systems in the The irregular plane of breakability is the function of mixing
vitrain bands. In contrast, the Barakar Formation coal samples organo−inorganic content and alternate deformed heteroge-
show deformed cleat/fracture, which lost the original structures neous bands (Figure 5n). The irregular cracks and well-
due to heat effects, basin tectonics, higher compaction, and developed face and butt cleats in vitrain indicating postdeposi-
thermal transformation. The thick vitrain band is shown in the tional tectonics are responsible for cleat genesis in coal (Figure
horizontal sections of sample no. CG-1901; its schematic and 5o,p). The master cleat at the center with a high density of face
vertical section indicate the higher intensity of both the face and and butt cleat is shown in Figure 5q. It is interpreted that there is
butt cleat. The face and butt cleat are the properties of the vitrain no movement along the master cleat demonstrated by the face
lithotype because of the higher carbon content and brittle cleat. Likewise, the sample CG-1924 indicated partially
characteristics, specifying that the coal seam was subjected to deformed intensified cleat and cracks during postdepositional
constant stresses (Figure 5a).4,47,48 Likewise, in CG-1902, the activities (Figure 5r). The impact of bituminization and thermal
bands of vitrain are slightly thick and contain multiple faces and transformation on cleat occurrence is shown in Figure 5s−t. The
butt cleats with a bright luster and subconchoidal fractures. The multiple influences on cleat consistency are demonstrated in
butt cleats are not always perpendicular to the face cleats (Figure Figure 5u,v. It is summarized that the depositional environment,
5b). Crowded face cleats in vitrain bands with irregular butt lithotype, type of organic matter, gelification extent, and tectonic
cleats with layers of fusain bands are present in the CG-1903 coal activities of the basin played an essential role in cleat generation.
sample with a master cleat traversing all of the bands (Figure 5c). Additionally, the change in bedding plane orientation and
The cleats in coal sample no. CG-1904 are in a thick band of thermal compaction also supported the formation of the cleat.
vitrain with a broad face and butt cleats. These cleats are inclined 3.3. Role of Geochemical Attributes in Cleat/Fracture.
to the core axis, and at some part, the coal sample parted away The analyses data on the proximate properties of the Barakar
along with the major cleats (Figure 5d). Coal sample nos. CG- Formation coal samples like moisture (IM), ash, volatile matter
1917 and CG-1931 show secondary cleat infilling with (VM), and fixed carbon (FC) content are in the range of 0.92−
calcareous materials. It has been observed that if the vitrain 3.04 wt % (avg. 1.50 wt %; stdev. 0.59); 12.05−24.68 wt % (avg.
band is thick, the face and butt cleats are widely developed 18.67 wt %; stdev. 4.23), 16.11−28.48 wt % (avg. 22.28 wt %;
compared to the thin vitrain bands. stdev. 4.12), and 46.92−70.83 wt % (avg. 57.54 wt %; stdev.
Similarly, the Barakar coal samples, from sample nos. CG- 7.74), respectively (Table 4). The low moisture content,
1905 to CG-1915 (Figure 5e−k), show distorted, asymmetrical, significant carbon content, and moderate values of the volatile
crumpled, uneven cleats with a vitreous gellified luster, matter when placed in Seyler’s diagram illustrate the thermally
indicating that the constituents of coal passed through a plastic matured medium-volatile coal of bituminous rank. The fuel ratio
state caused by a thermal process due to nearby igneous (FR; the ratio of volatile matter to fixed carbon) varies from 1.73
intrusions.49 Tertiary cleats are seen to develop in coal sample to 4.40 (avg. 2.72; stdev. 0.84), also indicating the carbon-rich
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Table 4. Borehole Location, Formation Type, and Proximate and Ultimate Analyses Results of Coal Samples
proximate analysis (wt %) ultimate analysis (wt %) atomic ratio
coal-bearing
formation borehole ID depth fuel
and contacts and location sample no. (m) IM Ash VM FC ratio C H N S O O/C H/C
Raniganj BH#01, CG-1901 221 6.96 11.78 16.75 64.51 3.85 60.01 8.54 1.93 0.01 17.73 0.39 0.17
Ichhapur
CG-1902 283 6.35 15.66 21.47 56.52 2.63 57.83 10.48 1.93 0.01 14.09 0.32 0.22
CG-1903 318 6.40 17.23 25.20 51.17 2.03 56.89 12.43 1.98 0.01 11.46 0.27 0.26
CG-1904 392 6.12 16.36 22.28 55.24 2.48 57.55 9.81 1.97 0.01 14.30 0.33 0.21
Barakar BH#02, CG-1905 565 1.66 12.50 20.12 65.72 3.27 61.84 10.85 2.08 0.02 12.72 0.27 0.21
Sitarampur
CG-1906 830 1.72 20.57 28.48 49.23 1.73 55.07 13.73 2.43 0.02 8.18 0.20 0.30
CG-1907 869 1.01 12.05 16.11 70.83 4.40 65.62 8.20 2.20 1.71 10.22 0.21 0.15
Barakar BH#03, CG-1908 481 1.74 19.09 27.79 51.38 1.85 51.48 12.65 2.04 1.59 13.15 0.34 0.30
Sitarampur
CG-1909 660 1.23 17.40 23.59 57.78 2.45 57.63 11.16 2.13 1.49 10.19 0.24 0.23
CG-1910 728 1.59 24.68 26.81 46.92 1.75 52.57 15.98 2.34 1.78 2.65 0.07 0.37
CG-1911 768 1.19 22.47 18.87 57.47 3.05 61.33 10.92 2.30 1.79 1.19 0.03 0.22
Barakar BH#04, CG-1912 943 3.04 24.56 23.73 48.67 2.05 53.15 13.59 2.13 1.63 4.94 0.12 0.31
Kulti
CG-1913 968 1.15 18.29 19.45 61.11 3.14 60.56 8.66 2.21 1.71 8.57 0.19 0.17
CG-1914 1029 0.92 17.28 21.57 60.23 2.79 62.90 12.70 2.17 1.72 3.23 0.07 0.24
CG-1915 1048 1.26 16.51 18.61 63.62 3.42 61.72 9.22 2.23 1.73 8.59 0.19 0.18
Raniganj BH#05, CG-1916 323 7.49 20.34 28.70 43.47 1.51 52.55 11.36 2.03 1.40 12.32 0.31 0.26
Trans
Damodar
CG-1917 412 5.21 18.09 20.68 56.02 2.71 59.85 10.41 1.99 1.37 8.29 0.18 0.21
CG-1918 508 5.12 17.42 21.65 55.81 2.58 60.44 10.98 2.03 1.42 7.71 0.17 0.22
CG-1919 596 4.95 28.40 29.21 37.44 1.28 49.80 16.72 2.02 0.26 2.80 0.08 0.41
Raniganj BH#06, CG-1920 275 5.29 22.08 31.42 41.21 1.31 53.87 12.79 1.97 0.26 9.03 0.22 0.29
Andal
CG-1921 500 4.50 17.47 16.87 61.16 3.63 57.47 10.50 1.98 0.27 12.31 0.29 0.22
CG-1922 560 4.27 13.86 25.96 55.91 2.15 53.09 14.54 1.98 0.28 16.26 0.41 0.33
CG-1923 632 4.10 15.75 27.82 52.33 1.88 58.83 13.99 1.96 0.27 9.20 0.21 0.29
Raniganj BH#07, CG-1924 178 7.31 24.33 27.96 40.40 1.44 49.91 14.57 2.04 0.25 8.90 0.24 0.35
Jagannath
pur,
Durgapur
CG-1925 270 7.95 20.95 28.04 43.06 1.54 52.05 11.01 2.04 0.25 13.70 0.35 0.26
CG-1926 282 7.23 24.86 26.64 41.27 1.55 56.66 10.71 2.07 0.26 5.44 0.13 0.23
CG-1927 358 7.88 19.42 28.29 44.41 1.57 53.11 11.41 2.03 0.25 13.78 0.35 0.26
Raniganj BH#08, CG-1928 151 4.97 22.83 32.95 39.25 1.19 48.80 16.10 1.94 0.27 10.06 0.27 0.40
(CH-10)
CG-1929 295 4.91 20.63 33.04 41.42 1.25 49.52 16.73 1.98 0.27 10.87 0.29 0.41
CG-1930 337 3.93 17.85 31.97 46.25 1.45 54.47 15.51 1.96 0.27 9.94 0.24 0.34
CG-1931 556 4.24 21.69 26.07 48.00 1.84 56.01 14.30 2.16 0.29 5.55 0.13 0.31
Raniganj maximum 7.95 28.40 33.04 64.51 3.85 60.44 16.73 2.16 1.42 17.73 0.41 0.41
coal
minimum 3.93 11.78 16.75 37.44 1.19 48.80 8.54 1.93 0.01 2.80 0.08 0.17
average 5.76 19.35 26.15 48.74 1.99 54.94 12.64 2.00 0.38 10.69 0.26 0.28
stdev. 1.34 4.01 4.86 8.01 0.77 3.74 2.48 0.05 0.45 3.77 0.09 0.07
Barakar coal maximum 3.04 24.68 28.48 70.83 4.40 65.62 15.98 2.43 1.79 13.15 0.34 0.37
minimum 0.92 12.05 16.11 46.92 1.73 51.48 8.20 2.04 0.02 1.19 0.03 0.15
average 1.50 18.67 22.28 57.54 2.72 58.53 11.61 2.21 1.38 7.60 0.18 0.24
stdev. 0.59 4.23 4.12 7.74 0.84 4.79 2.39 0.12 0.68 4.06 0.09 0.07
bituminous coal. Similarly, the Raniganj Formation coal proximate properties reveal that the Barakar coals are more
constituents like moisture (IM), ash, volatile matter (VM), matured than Raniganj coals because they are geologically older,
fixed carbon (FC) content, and fuel ratio are in the range of occurs at greater depth, and have passed through longer
3.93−7.95 wt % (avg. 5.76 wt %; stdev. 1.34), 11.78−28.40 wt % coalification processes.37,50
(avg. 19.35 wt %; stdev. 4.01), 16.75−33.04 wt % (avg. 26.15 wt The results of ultimate analyses (CHNSO) of Barakar coal
%; stdev. 4.86), 37.44−64.51 wt % (avg. 48.74 wt %; stdev. were in the range of 51.48−65.62 wt % (avg. 58.53 wt %; stdev.
8.01), and 1.19−3.85 (avg. 1.99; stdev. 0.77), respectively 4.79), 8.20−15.98 wt % (avg. 11.61 wt %; stdev. 2.39), 2.04−
(Table 4). The Raniganj Formation coal can be categorized as 2.43 wt % (avg. 2.21 wt %; stdev. 0.12), 0.02−1.79 wt % (avg.
carbon-rich with medium- to high-volatile bituminous rank. The 1.38 wt %; stdev. 0.68), and 1.19−13.15 wt % (avg. 7.60 wt %;
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stdev. 4.06), respectively, for carbon, hydrogen, nitrogen, sulfur, The evolutionary path of types III−IV kerogen is shown by
and oxygen (Table 4). The values of atomic ratios of H/C and the van Krevelen plot of H/C and O/C atomic ratios of studied
O/C vary from 0.03 to 0.34 (avg. 0.18; stdev. 0.09) and from coals, indicating a humic nature (Figure 7). It has also been
0.15 to 0.37 (avg. 0.24; stdev. 0.07), respectively. Likewise, the
results of carbon, hydrogen, nitrogen, sulfur, and oxygen
contents of Raniganj coal are in the range of 48.80−60.44 wt
% (avg. 54.94 wt %; stdev. 3.74), 8.54−16.73 wt % (avg. 12.64 wt
%; stdev. 2.48), 1.93−2.16 wt % (avg. 2.00 wt %; stdev. 0.05),
0.01−1.42 wt % (avg. 0.38 wt %; stdev. 0.45), and 2.80−17.73 wt
% (avg. 10.69 wt %; stdev. 3.77), respectively (Table 4). The
values of atomic ratios of H/C and O/C vary from 0.08 to 0.41
(avg. 0.26; stdev. 0.09) and from 0.17 to 0.41 (avg. 0.28; stdev.
0.07), respectively. The high carbon and hydrogen values in
Raniganj Formation coals also confirm the carbon-rich high-
volatile coals of bituminous rank. The Box and Whisker plot
shows the range of proximate and CHNSO constituent
distributions in studied coal core samples (Figure 6). The
narrow range of variation indicated by moisture content, volatile
matter, carbon, and oxygen reveals that Barakar coal is
comparatively matured than Raniganj coals. However, a little
variation in the carbon, hydrogen, and oxygen contents is Figure 7. van Krevelen plot of H/C and O/C atomic ratios showing
demonstrated by the heterogeneity in the organo−inorganic kerogen type in coal samples.
content, depositional conditions, and thermal maturity.
supported by the predominance of a vitrain lithotype and
alternate bright and dull bands.30,51,52 It is interpreted that both
the Raniganj and Barakar coals are subjected to organic thermal
transformation by the basin sinking and heavy load of
overburden sediments in a long geological period. Relatively
low H/C and O/C ratios may be described by continuous
reduction of the hydrogen content due to the compaction and
coalification process, which is also responsible for the cleat
genesis as a function of loss of plasticity. The relationships of
megascopic cleat intensity with proximate and ultimate
constituents are presented in Figure 8a−f. The inverse relation
of volatile matter with master, face, and butt cleats with good
correlation coefficients (R2 = 0.7899, 0.5106, and 0.5396)
postulates that higher thermal maturity increases the cleat
intensity as a function of loss of organic oil by thermal
compaction (Figure 8a). The carbon enrichment in coal during
maturation controls the megascopic cleat genesis pattern
(Figure 8b,c). The vitrain-rich bands of coal having high carbon
are more prone to cleat formation due to their brittle
characteristics. The hydrogen content in coal is also an indicator
of the type of coal. The reduction of hydrogen content during
organic matter transformation is also responsible for cleat
genesis (Figure 8d). The relation of O/C and H/C with
megascopic cleat intensity (Figure 8e,f) signifies primary
thermal compaction, mainly accountable for cleat genesis in
coal.
3.4. Organo-Petrographic Characteristics and Depo-
sitional Environment. The maceral composition of coal has
been measured in detail to delineate organic facies, microscopic
cleat, and microlithology and to deduce the paleo-environments
and hydrodynamic conditions deposition. The studied samples
show the presence of all three maceral groups; the values of
different maceral and mineral matters are listed in Table 5, and
microphotographs are shown in Figure 9a−p. The vitrinite
group recorded a higher concentration (avg. 44.02 vol % on
mineral matter free basis (mmf)) and is mainly dominated by
collotelinite maceral (avg. 35.86 vol %), while tellinite is trivially
Figure 6. Box and Whisker plot showing the content range of proximate present and is included in collotelinite values. The detrovitrinite
and CHNSO constituents in coal samples (B, Barakar; R, Raniganj; B & subgroup (avg. 5.07 vol %) has been recorded in lesser
R, Barakar and Raniganj combined). concentrations and is represented by vitrodetrinite and
K https://doi.org/10.1021/acsomega.1c02041
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sample no. collotelinite detrovitrinite sporinite cutinite resinite liptodetrinite semifusinite fusinite inertodetrinite (MM) vol % vitrinite liptinite inertinite TPI GI VI GWI VRom
CG-1901 32.99 8.15 13.24 3.26 3.05 5.50 18.94 1.23 10.79 2.85 42.35 25.78 31.87 2.81 1.09 2.98 0.33 1.24
CG-1902 32.87 9.99 15.87 2.50 4.99 6.12 13.15 5.67 6.58 2.26 43.85 30.16 25.99 3.12 1.30 3.31 0.37 1.37
CG-1903 29.76 7.35 13.00 1.68 5.24 6.29 10.48 4.20 10.48 11.52 41.94 29.62 28.44 2.49 1.17 2.67 0.63 1.26
CG-1904 43.40 4.55 11.36 2.73 1.59 7.27 11.36 0.92 6.36 10.46 53.55 25.63 20.82 5.10 2.22 3.93 0.35 1.47
CG-1905 30.34 3.68 3.68 0.92 5.75 10.34 20.22 5.29 8.05 11.73 38.54 23.44 38.02 4.76 0.86 3.00 0.51 1.32
CG-1906 32.72 0.69 4.35 2.29 2.75 7.09 9.15 17.85 14.65 8.46 36.50 18.00 45.50 3.89 0.80 3.08 0.28 1.62
CG-1907 31.40 - 1.84 0.53 3.96 13.72 29.82 4.22 11.87 2.64 32.25 20.59 47.15 5.51 0.68 2.80 0.08 1.55
CG-1908 38.89 1.21 13.04 3.38 3.39 6.28 18.11 3.38 8.94 3.38 41.50 27.00 31.49 5.95 1.25 4.88 0.12 1.65
CG-1909 25.57 1.77 1.77 1.77 5.57 8.61 31.13 6.08 10.38 7.35 29.51 19.13 51.37 5.17 0.54 3.46 0.36 1.18
CG-1910 31.47 5.17 2.59 0.00 5.17 13.79 10.77 6.47 9.48 15.09 43.15 25.38 31.47 3.32 1.07 1.99 0.64 1.39
CG-1911 34.19 4.41 1.10 0.37 4.41 8.46 29.41 5.15 6.62 5.88 41.01 15.24 43.75 6.23 0.75 3.83 0.30 1.25
CG-1912 32.87 1.11 2.94 0.68 8.36 6.96 25.90 2.23 13.37 5.58 35.99 20.06 43.95 4.17 0.75 3.40 0.20 1.15
CG-1913 35.19 3.29 2.96 0.32 5.82 8.37 22.79 4.30 9.62 7.34 41.53 18.85 39.62 4.82 0.88 3.35 0.30 1.40
CG-1914 36.23 2.23 0.74 0.00 2.23 8.44 25.31 2.24 15.63 6.95 41.33 12.26 46.41 3.57 0.80 2.54 0.25 1.16
CG-1915 34.44 3.83 0.50 0.00 2.05 2.30 34.44 2.55 14.80 5.09 40.32 5.11 54.57 3.83 0.63 3.53 0.26 1.63
CG-1916 33.33 5.03 13.84 4.40 2.52 4.82 13.21 0.62 14.47 7.76 41.59 27.73 30.68 2.42 1.00 2.79 0.38 1.22
CG-1917 28.57 3.15 20.34 4.60 1.45 3.15 13.08 0.73 15.25 9.68 35.12 32.71 32.17 2.29 1.07 3.19 0.45 1.31
CG-1918 29.62 4.90 14.25 1.79 1.11 4.23 19.38 3.56 11.36 9.80 38.27 23.70 38.03 3.23 0.85 3.40 0.50 1.30
M
CG-1919 39.20 5.57 15.37 5.79 0.67 4.01 12.03 1.56 12.25 3.55 46.42 26.79 26.79 2.96 1.38 3.42 0.23 1.19
CG-1920 35.87 7.61 13.48 5.00 2.17 1.96 13.48 1.52 11.30 7.61 47.06 24.47 28.47 2.69 1.28 3.43 0.42 0.98
CG-1921 36.84 10.04 9.15 1.34 1.79 5.13 14.96 1.78 8.93 10.04 52.11 19.35 28.53 2.82 1.24 2.73 0.55 1.36
CG-1922 41.98 5.27 11.21 1.97 0.88 4.62 15.82 5.28 10.33 2.64 48.53 19.19 32.28 4.04 1.25 3.82 0.19 1.33
CG-1923 42.62 4.60 9.93 2.66 0.97 7.02 11.86 0.98 10.65 8.71 51.73 22.54 25.73 3.64 1.68 3.10 0.31 1.46
http://pubs.acs.org/journal/acsodf
CG-1924 31.52 6.58 10.20 2.95 1.36 5.22 15.87 1.82 16.78 7.70 41.28 21.38 37.35 2.09 0.92 2.23 0.45 1.11
CG-1925 34.90 3.88 12.86 2.87 1.83 5.91 12.65 1.43 11.84 11.83 43.98 26.62 29.40 3.12 1.25 3.08 0.45 1.29
CG-1926 37.85 7.86 11.67 2.62 0.71 5.71 16.43 3.57 8.81 4.77 48.00 21.75 30.25 3.46 1.29 3.26 0.33 1.32
CG-1927 37.96 8.46 11.71 4.13 1.08 3.47 18.22 2.39 9.11 3.47 48.09 21.12 30.79 3.33 1.32 3.59 0.31 1.47
CG-1928 46.58 5.56 13.89 2.57 0.85 4.27 10.90 1.92 6.62 6.84 55.97 23.16 20.87 4.88 2.02 4.66 0.27 1.02
CG-1929 47.40 7.36 12.12 7.14 1.30 3.25 6.28 1.94 5.63 7.58 59.25 25.76 14.99 4.28 3.12 4.69 0.32 1.08
CG-1930 44.27 5.83 9.90 6.02 3.11 6.21 6.99 3.88 7.38 6.41 53.53 26.97 19.50 4.17 2.45 3.82 0.28 0.94
CG-1931 40.67 2.94 12.16 2.93 4.82 7.76 3.77 2.73 9.01 13.21 50.25 31.88 17.87 3.95 2.36 3.40 0.40 1.29
max 47.40 10.04 20.34 7.14 8.36 13.79 34.44 17.85 16.78 15.09 59.25 32.71 54.57 6.23 3.12 4.88 0.64 1.65
min 25.57 0.69 0.50 0.00 0.67 1.96 3.77 0.62 5.63 2.26 29.51 5.11 14.99 2.09 0.54 1.99 0.08 0.94
avg 35.86 5.07 9.39 2.56 2.93 6.33 16.64 3.47 10.56 7.36 44.02 22.95 33.04 3.81 1.27 3.33 0.35 1.30
stdev. 5.43 2.52 5.45 1.87 1.98 2.80 7.66 3.16 3.01 3.35 6.99 5.73 9.93 1.09 0.60 0.65 0.13 0.18
Article
Figure 9. Micropetrographic photographs showing microlithotype, maceral types, and microscopic cleat in coal samples.
Table 6. Cleat/Fracture Intensity and Spacing Measured on Different Visualization Scales in Coal Samples
megascopic (in 100 cm2) microscopic (in 6.25 cm2) scanning electron microscopy (in 1 mm2)
cleat intensity (%) cleat intensity (%) cleat spacing (μm) cleat intensity (%) cleat spacing (μm)
sample no. MCL FCL BCL <2 2−5 >5 <10 10−20 >20 <5 5−10 >10 <2 2−5 >5
CG-1901 3.85 16.23 7.21 3.11 3.16 3.08 2.23 10.19 20.19 3.85 8.23 9.76 0.54 2.04 6.23
CG-1902 3.06 15.37 6.58 2.64 3.26 3.16 3.63 11.91 25.05 3.97 7.64 8.09 1.06 2.78 8.65
CG-1903 2.15 7.91 5.23 1.17 3.07 3.06 6.75 12.64 23.76 3.36 6.45 7.85 1.07 2.94 9.52
CG-1904 2.75 11.87 4.29 1.74 2.48 1.98 7.54 13.92 31.56 3.16 5.36 5.49 1.48 3.58 14.23
CG-1905 2.61 14.32 6.45 1.72 2.82 2.91 4.77 10.43 20.25 3.9 7.25 7.92 1.02 2.76 7.56
CG-1906 1.14 5.17 2.49 0.98 2.63 1.33 7.69 14.25 32.92 2.49 6.32 6.33 1.63 3.79 12.22
CG-1907 3.56 17.29 6.18 3.46 3.78 2.46 4.26 10.68 23.35 3.63 7.2 8.25 0.78 2.45 5.46
CG-1908 1.21 13.61 4.25 0.95 1.97 3.12 4.33 13.63 26.26 3.41 6.79 6.37 1.07 3.56 6.45
CG-1909 1.58 11.23 3.85 1.66 2.95 0.95 5.94 14.85 24.59 3.46 6.85 5.26 1.55 3.05 17.3
CG-1910 0.85 6.28 3.96 1.79 2.61 1.65 7.85 15.25 32.27 2.85 5.69 8.01 1.61 3.85 18.26
CG-1911 2.26 9.36 6.78 2.34 2.36 1.42 5.29 10.94 25.18 3.28 5.78 7.68 1.36 2.62 13.48
CG-1912 1.47 6.32 2.88 1.48 2.24 1.96 6.58 13.36 28.5 2.58 6.4 4.92 1.24 3.58 14.67
CG-1913 3.04 16.95 5.78 2.15 3.26 2.57 4.21 10.78 22.69 3.7 8.65 8.34 0.76 2.94 8.62
CG-1914 2.21 8.91 4.48 1.59 2.12 1.39 4.68 10.36 24.71 3.48 7.29 7.05 1.12 2.79 9.27
CG-1915 2.86 17.29 5.65 1.64 3.16 2.56 5.02 11.49 25.28 3.55 8.5 8.34 0.78 2.22 8.37
CG-1916 1.75 11.62 3.51 2.49 2.23 1.55 6.56 12.77 28.95 3.46 6.41 9.16 1.23 3.79 9.94
CG-1917 3.31 13.46 6.14 3.36 2.33 2.16 6.37 11.26 23.52 3.24 5.46 7.13 1.33 2.85 14.33
CG-1918 2.58 14.78 4.82 2.58 2.21 2.3 6.26 14.38 30.13 2.53 8.26 6.77 1.21 3.39 17.25
CG-1919 0.62 5.96 3.26 1.46 1.65 1.47 7.35 14.92 35.85 2.55 5.47 4.63 1.65 3.74 16.59
CG-1920 1.45 8.39 3.44 1.75 2.12 1.96 5.64 14.56 31.27 2.92 6.85 7.26 1.12 3.14 14.85
CG-1921 3.11 14.62 4.45 1.59 2.26 3.49 5.15 11.21 29.36 3.33 7.89 8.65 1.26 2.64 11.59
CG-1922 1.69 10.29 5.16 1.85 3.36 1.88 5.04 12.62 28.25 3.48 7.78 9.26 1.36 3.35 10.36
CG-1923 2.17 12.26 5.69 4.02 3.22 2.46 4.45 11.23 21.56 3.63 7.79 7.11 1.22 2.96 8.22
CG-1924 1.26 5.47 4.16 1.25 2.31 1.49 5.26 14.61 32.73 3.09 5.64 5.58 1.95 3.46 14.26
CG-1925 1.94 8.28 3.78 1.56 2.16 1.78 6.99 12.8 27.91 2.89 6.56 6.84 1.16 3.98 15.89
CG-1926 1.87 13.62 4.04 1.95 2.85 2.55 5.88 10.39 27.35 2.95 5.62 7.25 0.85 3.47 9.33
CG-1927 1.75 12.36 6.19 1.84 4.12 2.16 4.71 11.73 22.29 3.61 7.26 9.26 1.12 2.69 7.63
CG-1928 0.36 3.85 3.14 0.49 1.26 1.04 6.55 14.91 35.79 2.59 6.85 5.74 1.26 4.06 14.22
CG-1929 0.47 5.9 1.65 1.08 1.44 0.65 6.28 15.58 36.49 2.07 5.11 5.88 1.86 4.48 19.18
CG-1930 0.72 7.62 1.83 1.64 1.88 1.02 7.46 16.27 34.08 2.11 5.26 4.68 1.88 4.66 15.64
CG-1931 1.38 4.36 4.29 1.22 1.53 1.22 8.05 13.65 28.32 2.64 6.42 8.21 1.53 3.55 14.29
max 3.85 17.29 7.21 4.02 4.12 3.49 8.05 16.27 36.49 3.97 8.65 9.76 1.95 4.66 19.18
min 0.36 3.85 1.65 0.49 1.26 0.65 2.23 10.19 20.19 2.07 5.11 4.63 0.54 2.04 5.46
avg 1.97 10.68 4.57 1.89 2.54 2.03 5.77 12.82 27.76 3.15 6.74 7.20 1.26 3.26 12.06
stdev. 0.94 4.16 1.45 0.79 0.68 0.75 1.39 1.83 4.68 0.52 1.03 1.43 0.34 0.63 3.93
The SEM cleat spacings show an inverse relation with quartz are also observed (Figure 17a−h), suggesting a quartz-
microscopic intensity. It suggests that microstresses related to rich source rock. Consequently, the occurrence of a large
compaction, dehydration, devolatilization, and internal shrink- amount of quartz in the samples suggests the brittle nature of
age/desiccation played a vital role in cleat genesis (Figure 16d,f). coal, which may help establish the connectivity between the
3.6. Influence of Mineral Constituents on Cleat/ fracture and pores during hydrofracturing in coal seam gas
Fractures. The X-ray diffraction (XRD) spectrum is a reliable reservoirs.72 Usually, quartz grains are relatively more resilient to
tool for identifying different mineral/inorganic compositions in the weathering agents compared to K-feldspar. Therefore, the
coal samples and understanding the source rock properties.34−36 stress fields of burial depth, geothermal gradient, and textural
The values of the identified mineral phases in the studied alterations due to diagenesis have a negligible influence.30,35,36
samples are enumerated in Table 7. The patterns of XRD spectra The evaluation of clay mineral types from XRD can help
(Figure 17a−g) revealed that the studied samples possess reconstruct the environmental conditions prevailing during
nonclay minerals predominantly (47.42−83.95 vol %), includ- sedimentation. It appears that the presence of kaolinite in the
ing quartz (21.66−57.14 vol %), clintonite (1.00−23.53 vol %), studied coal seams reveals intense leaching of inorganic minerals
and calcite (2.56−13.32 vol %). Other nonclay minerals such as (feldspar and pyroxene) in an acidic medium under a humid-
dolomite (2.56−17.66 vol %), muscovite (0.25−8.41 vol %), fluvio-terrestrial climate.73 Illite, on the other hand, usually
and pyrite (0.12−1.25 vol %) were found at relatively lower forms in a relaxed environment under low precipitation.
concentrations. The clays are second in abundance and range Meunier,74 however, advocates that an arid environment with
from 16.05 to 52.58 vol %. Among them, dickite and kaolinite a weak eluvial process is more suitable for forming and
range from 2.95 to 16.67 vol % and from 3.31 to 46.52 vol %, preserving illites. The formation of kaolinite and illite can be
respectively, while illite is recorded up to 14.96 vol %. The data attributed to the weathering of silicates like mica and feldspar
show that, in general, the more prominent XRD peaks of quartz minerals. It is also formed due to the alteration of smectite and
are noted in all of the samples although some small peaks of other minerals (muds and silts) during diagenesis. The larger
P https://doi.org/10.1021/acsomega.1c02041
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Figure 13. Relationship of cleats in coal samples. (a) Master cleat intensity vs face and butt cleat intensities. (b) Master cleat vs microscopic cleat
intensity. (c) Face cleat vs microscopic cleat intensity. (d) Butt cleat vs microscopic cleat intensities.
Figure 15. Relationship of lithotype intensities with cleat intensities of coal samples. (a) VRom vs B (bright coal). (b) VRom vs Db (dull banded coal).
(c) Megascopic cleat intensity vs B (bright coal). (d) Microscopic cleat spacing vs B (bright coal). (e) Megascopic cleat intensity vs Db (dull banded
coal). (f) Microscopic cleat intensity vs Db (dull banded coal). (g) SEM cleat intensity vs Db (dull banded coal). (h) SEM cleat spacing vs Db (dull
banded coal).
through strong weathering patterns and are elastic in nature and desorption branches of the isotherms show distinct
(Figure 18l). hysteresis loops in almost all of the samples except for sample
3.7. Matrix-Associated Pore Types in Coal. The low- nos. CG-1906 to CG-1909, CG-1922, CG-1923, CG-1928, and
pressure N2 adsorption−desorption isotherm curves are used to CG-1929. The negligible hysteresis pattern indicates less
determine the surface area, pore size, pore volume, and coal condensation of gas in the mesopores. The dominance of slit,
matrix pore structures. The types of pores, the pore volume, and combined, and open-ended cylindrical pores is associated with
the surface area of coals are essential to determine the gas cleat and fracture systems. The reduction in adsorption of gas
holding capacity. The fluid flow mechanism of the coal seam is with increasing relative pressure (sample nos. CG-1910 and
due to adsorption, and the desorption from the internal surfaces 1927) indicates condensation of gas after filling the monolayer
is a function of the pore type and pore volume.78 The isotherms and multilayer due to the abundance of large cylindrical open
obtained from the N2 sorption study of the studied coal samples pores in the samples (Figure 19e).
correspond to the types-I and II isotherms with desorption The surface area, pore size, and pore volume were obtained
hysteresis pattern Types A and B, which are characteristics of a from the low-pressure nitrogen (N2) sorption isotherm curves
well-developed mesopore having cylindrical, slit-shaped, and following different methods (Table 8). The multipoint BET
combined open pores (Figure 19a−j).37,79−81 The adsorption surface area, the Barrett−Joyner−Halenda (BJH) pore volume,
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Figure 16. Relationship of cleats with thermal maturity (VRom%) of coal samples. (a) VRom vs depth. (b) Megascopic cleat intensities vs VRom. (c)
Microscopic cleat intensities vs VRom. (d) Microscopic cleat spacing vs VRom. (e) SEM cleat intensities vs VRom. (f) SEM cleat intensities vs VRom.
and pore size distributions vary from 1.352 to 14.348 m2/g, 3.8. Microfractures and Pore Morphology in Coal. The
0.002 to 0.021 cm3/g, and 2.057 to 13.320 nm, respectively. As field emission scanning electron microscopy (FE-SEM) photo-
per the International Union of Pure and Applied Chemistry graphs (Figure 22a−p) of the Raniganj and Barakar Formations
(IUPAC), the pores of coal can be grouped into three types: ≥50 coal seams show intricate microfractures and pore structures
nm (macropores), 2−50 nm (mesopores), and ≤2 nm owing to the epigenetic characteristics. It also indicates that only
(micropores).82 The BJH plots indicate the dominance of vitrinite bands comprise the partially deformed planer cleat
mesopores in studied coal samples (Figure 20a−l). Generally, system (Figure 22a). These cleats and fractures are the main
the pore structure plays a vital role in the flow of fluid in the pathways for the movement of gas through the coal. The
interlinked dendritic pore to the cleat/fracture coal system. diversified pore system can be observed in microlithotypes like
The vitrinite content showed an increasing trend with clarite, inertite, and durite containing macerals, e.g., collotelinite,
increasing multipoint BET surface area, signifying that pores detrovitrinite, fusinite, semifusinite, and mineral matters (Figure
associated with the vitrinite maceral mainly contributed to the 22b−d).84 Further, the quartz and clay grains having algae
total surface area (Figure 21a). Moreover, the vitrinite content overgrown developed shallow and deep micropores to
vs the BJH pore volume and pore size revealed a very good mesopores in coal (Figure 22e). Decomposed pores due to
correlation (R2 = 0.8118 and R2 = 0.7612, respectively) (Figure heat received from external intrusive altering microlithotypes are
21b,c). The pores and fractures in vitrinite-containing matrix shown in Figure 22f. It may be noticed that collotelinite, inertite,
systems having a carbon-rich lithotype merged to form clusters and dull bands have macro- and mesopores partially filled with
with irregular connections due to pre- and post-tectonic secondary clay minerals like illite and kaolinite (Figure 22g,h).
stresses.83 Figure 21d−f exhibits the relation of inertinite The evolution of organic pores by cracking organic compounds
content with multipoint BET surface area, BJH pore volume, during coalification is illustrated in Figure 22i. The sericite clay
and pore size, indicating the evolution of chiefly large-diameter having irregular altered micropores and cracks allied with
pores in the studied coals during inertinization or alteration of duroclarite is shown in Figure 22j,k. Distinct polymeric boghead
organic matter. algae overgrew in macropores of vitrite during the postdeposi-
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Table 7. Minerals and Clays Identified through XRD Spectroscopy of Coal Samples
minerals (vol %) clays (vol %)
sample no. quartz muscovite chloritoid clintonite calcite dolomite pyrite total mineral (vol %) dickite kaolinite illite total clays (vol %)
CG-1901 57.14 0.26 - 14.29 6.14 - 0.95 78.78 14.08 7.14 - 21.22
CG-1902 50.22 1.25 0.52 7.22 2.56 6.34 0.18 68.29 7.25 21.81 2.65 31.71
CG-1903 38.26 3.47 0.85 8.56 4.64 2.56 1.25 59.59 11.26 24.89 4.26 40.41
CG-1904 42.62 1.69 5.27 10.52 5.27 - 0.63 66.00 5.27 23.46 5.27 34
CG-1905 44.19 3.48 1.62 6.37 8.51 4.18 - 68.35 5.62 21.98 4.05 31.65
CG-1906 25.67 2.11 0.95 5.16 6.74 6.37 0.42 47.42 4.58 46.52 1.48 52.58
CG-1907 55.33 3.41 1.48 2.44 2.96 4.59 - 70.21 4.98 18.48 6.33 29.79
CG-1908 35.3 1.76 - 11.76 5.88 17.66 0.74 73.1 11.76 13.26 1.88 26.9
CG-1909 33.58 8.41 1.65 7.65 5.98 3.78 0.18 61.23 7.56 26.92 4.29 38.77
CG-1910 35.36 3.68 2.58 1.00 4.22 5.44 0.69 52.97 6.35 38.21 2.47 47.03
CG-1911 44.29 2.11 2.96 8.56 3.72 6.7 - 68.34 4.95 20.39 6.32 31.66
CG-1912 30.29 0.56 - 23.53 5.88 3.15 0.47 63.88 11.76 18.48 5.88 36.12
CG-1913 47.26 2.14 1.47 21.58 6.55 4.59 0.36 83.95 8.56 3.31 4.18 16.05
CG-1914 35.78 1.72 3.14 20.14 5.94 6.22 0.14 73.08 7.62 9.64 9.66 26.92
CG-1915 40.99 2.00 5.05 12.33 7.45 15 0.37 83.19 2.95 6.63 7.23 16.81
CG-1916 31.92 3.14 1.45 10.62 5.74 5.78 - 58.65 5.96 31.14 4.25 41.35
CG-1917 42.78 1.92 1.26 8.59 6.47 6.59 0.33 67.94 8.56 19.88 3.62 32.06
CG-1918 46.63 0.98 10.53 10.53 5.26 - 0.95 74.88 15.79 7.22 2.11 25.12
CG-1919 32.96 1.22 1.74 7.56 5.95 4.29 1.22 54.94 4.36 36.47 4.23 45.06
CG-1920 34.25 3.47 1.56 5.98 7.21 6.47 0.48 59.42 8.65 25.61 6.32 40.58
CG-1921 44.42 1.22 5.56 11.11 5.56 5.56 0.12 73.55 14.78 9.22 2.45 26.45
CG-1922 40 0.34 3.05 6.67 13.32 4.73 0.47 68.58 12.24 15.86 3.32 31.42
CG-1923 38.95 0.75 3.66 7.59 4.99 5.51 0.62 62.07 4.63 30.97 2.33 37.93
CG-1924 33.68 0.36 3.58 14.25 3.44 6.15 - 61.46 8.56 28.57 1.41 38.54
CG-1925 30.17 1.74 3.96 8.69 6.51 7.24 0.37 58.68 5.64 29.36 6.32 41.32
CG-1926 41.43 1.65 5.56 11.11 11.10 - 0.69 71.54 16.67 6.23 5.56 28.46
CG-1927 45.77 1.89 2.45 4.89 7.25 5.95 - 68.20 8.95 18.00 4.85 31.8
CG-1928 28.99 0.25 2.75 9.55 4.96 4.58 0.72 51.80 4.96 31.01 12.23 48.2
CG-1929 21.66 0.65 11.3 4.34 12.30 3.08 0.31 53.64 6.66 35.07 4.63 46.36
CG-1930 23.47 1.74 2.85 10.45 5.88 5.48 0.58 50.45 7.22 27.37 14.96 49.55
CG-1931 30.37 1.25 5.26 10.53 10.53 5.26 - 63.20 10.53 21.01 5.26 36.80
maximum 57.14 8.41 11.30 23.53 13.32 17.66 1.25 83.95 16.67 46.52 14.96 52.58
minimum 21.66 0.25 0.52 1.00 2.56 2.56 0.12 47.42 2.95 3.31 1.41 16.05
average 38.18 1.96 3.36 9.79 6.42 6.05 0.55 65.08 8.35 21.75 4.99 34.92
stdev. 8.66 1.58 2.61 5.04 2.51 3.21 0.31 9.25 3.65 10.67 3.02 9.25
tional course (Figure 22l), creating an obstacle for pore dyke) control the microcleat/fracture and pore system in the
connectivity and the gas flow mechanism.85 The organic pores Raniganj and Barakar Formations coal seams.
that evolved during compaction, gelification, and thermal For more clarity on microcleats, the different microlithotypes
transformation generated deep irregular pores due to cracking observed under FE-SEM are revealed in Figure 23a. The vitrite
of organic compounds, as shown in Figure 22m. The parallelly showed a well-developed face and butt cleat perpendicular to
placed boghead algae in the microcleat blocking the flow path each other. The clarite indicates alternate thin bands, vertical
related to vitrite are illustrated in Figure 22n. The diatom (algae) fractures, and spacing aligning the beddings. The decomposed
in cracks/fractures indicates postdepositional overgrowth of altered organo−inorganic matter comprises mesopores and
algae by influencing the influx of water from nearby drainage fractures associated with durite and the parallel spacing-pores in
systems (Figure 22o). The deep pore (pore pipe) in clarain char formed during inertinization. It also validates the above
statement that maceral and geological transformation of organic
emphasizes lithotypes other than vitrinite, also expansively
matter influenced the pore, microcleat, and microfractures in
cracked and evolved large pores (Figure 22p). The micro-
coal.86,87 The micro- and mesopores in inertite-char on different
fractures linked with different pore structures in the studied coal magnifications (from 1.0 to 102.5k×) are shown in Figure 23b.
are classified into seven types: (i) vitrite-associated regular open- On zooming-in on the char bands, micro- and mesopores with
slit pores, (ii) vitriinertite-char allied irregular pores, (iii) connecting microfractures are gradually visible, demonstrating
irregular fracture pores partially filled with clay, (iv) fissile pores that inertodetrinite is transitional between vitrite and inertite.
along bedding planes of clay, (v) organic pores evolved due to This interaction is observed in the vitrite-clarite-inertite bands of
external heat received from intrusives, (vi) deep organic pores all of the studied coal samples. These microfractures look similar
evolved during compaction and thermal transformation, and to shrinkage cracks with ultrafine granularity developed in coal
(vii) pore fractures blocked by boghead algae. It is summarized due to dehydration.47,88−91
that the maceral type, microlithotype, diagenesis process, clay Similarly, the durite is magnified in four stages from 292× to
and mineral alteration, and heat received from intrusives (sill/ 37.65k× to determine the pore and fracture morphologies
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Figure 18. Relationship of cleat occurrence with mineral/clay content in coal samples. (a) Quartz content vs megascopic cleat intensity. (b) Total
mineral content vs megascopic cleat intensity. (c) Total clay content vs megascopic cleat intensity. (d) Quartz content vs microscopic cleat intensity.
(e) Quartz content vs SEM cleat intensity. (f) Total clay content vs microscopic cleat intensity. (g) Total clay content vs SEM cleat intensity. (h)
Quartz content vs microscopic cleat spacing. (i) Quartz content vs SEM cleat spacing. (j) Total clay content vs microscopic cleat spacing. (k) Total clay
content vs SEM cleat spacing. (l) Kaolinite content vs megascopic cleat intensity.
Figure 19. (a−j): Low-pressure N2 adsorption and desorption isotherm pattern showing cylindrical and slit-shaped pore types in the studied coal
samples.
investigated 31 coal samples from eight boreholes in the from organo−inorganic content and early diagenetic
Raniganj Coalfield by various measurements and analyses such effects to the coal late transformation process.
as petrography, proximate and ultimate analyses, X-ray ii. Face and butt cleat is the property of vitrain lithotypes
diffraction (XRD), low-pressure N2 sorption isotherm, cleat/ because higher carbon content and brittle characteristics
fracture intensity, and physicomechanical properties. The broad specifying the coal seam were subjected to uniform
stresses.
conclusions drawn from the study are as follows.
iii. The inverse relationship of volatile matter with master,
i. There are four distinct lithotypes identified: (i) B, bright face, and butt cleat thermal maturity controls the cleat
coal; (ii) Db, dull banded coal; (iii) Bb, bright banded intensity.
coal; and (iv) Bd, banded coal. These litho-facies iv. The carbon enrichment process in coal controls the
demonstrate color differences in lithotypes sourced megascopic cleat genesis pattern. The vitrain-rich bands
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Table 8. BET Surface Area, Pore Size, and Pore Volume Obtained through Low-Pressure N2 Adsorption of Coal Samples
surface area (m2/g) pore volume (cm3/g) pore size (nm)
sample no. single-point BET multipoint BET Langmuir BJH method t-method external BJH method DFT method BJH method DFT
CG-1901 1.162 2.626 2.013 0.694 1.226 0.004 0.003 4.489 3.969
CG-1902 2.453 2.663 4.287 1.910 2.663 0.007 0.006 5.189 5.689
CG-1903 2.133 1.509 3.446 0.821 0.987 0.010 0.003 4.262 0.718
CG-1904 4.314 4.379 8.971 2.778 4.379 0.014 0.007 9.450 3.627
CG-1905 3.285 1.352 6.767 2.515 3.852 0.005 0.007 2.057 3.969
CG-1906 2.022 5.499 4.621 1.581 2.093 0.004 0.003 3.161 2.769
CG-1907 3.883 6.410 42.060 3.947 3.589 0.004 0.006 1.988 2.769
CG-1908 4.840 3.320 23.320 4.387 4.904 0.004 0.008 2.989 3.169
CG-1909 2.308 2.495 4.124 1.167 1.446 0.002 0.003 1.993 0.718
CG-1910 0.401 5.644 0.597 0.278 0.644 0.004 0.002 5.070 1.410
CG-1911 3.057 3.691 7.403 2.105 3.533 0.008 0.006 3.160 2.769
CG-1912 2.133 2.452 4.292 1.471 2.452 0.005 0.005 3.486 2.769
CG-1913 3.290 2.960 0.320 5.820 12.790 0.006 1.200 5.794 4.820
CG-1914 1.232 1.719 3.336 1.690 1.719 0.004 0.003 3.341 1.410
CG-1915 0.864 10.887 2.926 0.563 0.887 0.009 0.001 4.346 2.769
CG-1916 5.991 6.638 23.050 3.747 3.980 0.007 0.007 2.990 3.169
CG-1917 5.476 13.867 15.860 3.650 4.488 0.005 0.008 3.203 3.627
CG-1918 1.862 8.041 3.466 1.260 2.041 0.006 0.005 3.161 3.969
CG-1919 1.991 12.826 3.484 1.100 2.082 0.010 0.004 7.991 3.969
CG-1920 2.054 6.329 4.097 1.150 1.995 0.012 0.004 5.993 3.169
CG-1921 1.211 7.443 2.792 0.592 0.987 0.016 0.002 10.160 3.169
CG-1922 11.990 10.330 35.140 9.937 10.150 0.013 0.017 5.989 3.169
CG-1923 9.673 12.370 46.010 8.650 8.969 0.015 0.016 8.085 3.169
CG-1924 4.322 14.607 7.158 2.305 4.607 0.008 0.011 4.492 3.969
CG-1925 1.461 12.587 2.583 0.876 1.587 0.008 0.005 5.460 4.543
CG-1926 2.381 10.883 3.569 1.508 1.888 0.014 0.011 13.320 7.795
CG-1927 0.515 11.206 0.747 0.659 1.206 0.010 0.004 5.739 3.969
CG-1928 8.277 13.096 14.730 4.344 4.421 0.021 0.009 10.991 0.718
CG-1929 6.510 14.348 12.580 4.520 5.110 0.017 0.009 11.285 2.897
CG-1930 4.682 12.330 14.520 3.876 4.464 0.015 0.007 11.159 2.769
CG-1931 8.184 9.416 15.950 6.023 7.576 0.013 0.013 7.728 3.627
maximum 11.990 14.607 46.010 9.937 12.790 0.021 1.200 13.320 7.795
minimum 0.401 1.352 0.320 0.278 0.644 0.002 0.001 1.988 0.718
average 3.676 7.546 10.459 2.772 3.636 0.009 0.045 5.759 3.259
stdev. 2.830 4.461 11.985 2.366 2.875 0.005 0.214 3.137 1.436
Figure 20. (a−l): BJH plot showing pore size distribution and cumulative pore volume in coal samples.
of coal with high carbon are more prone to cleat formation specifying that these cleats are interdependent and
due to their brittle characteristics. simultaneously developed during the thermal trans-
v. The hydrogen content in coal is also an indicator of coal formation of organic matter due to shrinkage, stress
type. The process of reduction of hydrogen content release, devolatilization, and extensional strain.
during organic matter transformation is also responsible
for cleat genesis. vii. The resistance to the weathering nature of quartz makes
vi. The master cleat (MCL) intensity is directly proportional its grains rounded to subrounded while transportation in
to face cleat (FCL) and butt cleat (BCL) intensities, the basin and contributes to the brittle properties of coal.
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Figure 23. (a−c): SEM photographs showing pore, cleat, and fracture
morphologies at focused points on different magnifications.
Figure 21. Relationship of macerals with surface area, pore size, and istics. Vitrinite bands indicate that it comprises the
pore volume of coal samples. (a) Vitrinite content vs multipoint BET partially deformed planer cleat system.
surface area. (b) Vitrinite content vs BJH pore volume. (c) Vitrinite ix. There is significant variation in strength properties of
content vs BJH pore size. (d) Inertinite content vs multipoint BET Barakar and Marren measures coal influenced by thermal
surface area. (e) Inertinite content vs BJH pore volume. (f) Inertinite maturity, lithotype characteristics, and organo−inorganic
content vs BJH pore size. content.
x. The positive relation between the quartz content and
This property makes coal easily breakable in a different Young’s modulus and Poisson’s ratio demonstrates that
direction by internal and external stresses. the increase in quartz content reduces the plasticity and
viii. The FE-SEM photographs show intricate microfractures more deformation occurs in coal. The relation between
and pore structures owing to the epigenetic character- the total clay content and Young’s modulus and Poisson’s
Figure 22. (a−p): SEM microphotographs showing variation in organic-matter-associated pores, fractures, minerals, and clays.
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ratio indicates the increase in elasticity with an increase in 5.2. Lithotype Analysis. The coal core samples were
the clay concentration in coal. studied megascopically for different lithotypes. Lithotypes in
bituminous coal are the most easily recognizable bands by the
naked eye and are described based on the distribution, amount,
5. MATERIAL AND METHODS and thickness of fibrous (charcoal), bright, and dull bands.92 has
classified the lithotypes of humic coal into four categories, i.e.,
5.1. Coal Sampling, Preparation, and Megascopic
vitrain, clarain, durain, and fusain; later, two more lithotypes
Cleat Intensity Measurement. A total of 31 sets of coal
samples were collected from eight exploratory boreholes drilled were introduced by Diessel,39 i.e., duroclarain and clarodurain.
at different locations in Raniganj Coalfield (Table 4; Figures 1 In this study, the classification proposed by Diessel38 is followed
and 2). The coal core samples were analyzed systematically for for lithotype identification of coal samples. The minimum
band-by-band with lithotype characteristics and the cleat thickness of the lithotype/band is considered to be 5 mm during
distribution in each band. The cleat/fractures were counted measurement (Tables 2 and 3).
along with length and types, and the megascopic cleat intensity 5.3. Proximate and Ultimate Analyses. The physical
was calculated for an area of 100 cm2. After determining the cleat attributes of coal (moisture, ash, volatile matter yield, and fixed
intensity, the coal core samples were crushed manually and carbon contents) were determined (in weight percentage) by
sieved (212 and 150 μm) for further analysis following the analyses performed on −212 μm-size coal samples, as per the
standard procedure as per the proximate and ultimate analyses procedure of the Bureau of Indian Standard.93 The elemental
and XRD requirement. Moreover, the samples were also compositions (carbon, hydrogen, nitrogen, sulfur, and oxygen)
prepared in size ranging from 0.8 to 1.0 mm for determining of the studied sample (−150 μm) were determined (in weight
the surface area, pellet preparation for petrographic character- percentage) using the Elementar Vario EL III-CHNS Analyzer
istics, and low-pressure N2 adsorption isotherm pattern using the standard procedure laid down by ASTM94−96 and IS.97
following the BET method. About 10 mg of prepared samples was taken and wrapped in a tin
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foil and then placed on the automatic sample stage of the CHNS
analyzer. The analyzer comprises an oxidation tube, a reduction
tube, and absorption columns for absorbing N2, CO2, SO2, and
water vapor. The amount of gases absorbed during oxidation
under the peaks was transformed into the elemental
configuration such as C, H, N, and S in the analyzer itself Figure 25. Box and Whisker plot showing range distribution of
through an inbuilt data acquisition program. The analysis results physicomechanical properties of coal samples (B, Barakar; R, Raniganj;
were presented in the data acquisition system connected to the B & R, Barakar and Raniganj combined).
analyzer after the input of required commands. The oxygen
amount was determined by subtracting the sum of C, H, N, S,
and ash from 100 (Table 4). through X-ray diffraction (XRD) by relating to the reference
5.4. Organic Petrography, Vitrinite Reflectance, and pattern values from the ICDD database. For the present study,
Microscopic Cleat/Fracture Analysis. The maceral analysis the analyses were carried out on a Rigaku−Ultima IV (Type II)
was carried out on pellets using a Carl Zeiss Axio Imager M2m X-ray diffractometer at CSIR-CIMFR, Dhanbad. The sample
microscope using 50×, simultaneously using white and preparation and the instrumental parameter mentioned in
fluorescence light modes and adopting the single-scan method. Mendhe et al.35 have been followed (Table 7).
The counting of the maceral was (1000 counts/sample) done on 5.6. Low-Pressure N2 Sorption Isotherm. The complex-
an automatic point counter stage of Petroglite 2.35 attached with ity and distribution of pore patterns were studied by low-
data acquisition software by following ICCP guidelines98 and pressure N2 sorption isotherms using the Quantachrome
subsequently adopted by ISO standards.99,100 The classification AutosorbiQ2 MP-XR machine at CSIR-CIMFR, Dhanbad.
and nomenclature were used as specified by the International The pore surface area, pore size, and pore volume of coal/shale
Committee for Coal and Organic Petrology101 for vitrinite, by BET techniques have been explained in several stud-
liptinite,102 and inertinite103 groups of macerals. The random ies.36,37,104,105 Coal samples of 40−50 mg and size 0.8−1 mm
vitrinite reflectance analyses were carried out on collotellinite were taken. To remove the moisture and residual gases, the coal
over 100 different points using a Carl Zeiss photomultiplier samples were degassed at 200 °C before the analysis. Nitrogen
(PMT) unit (Table 5). The microscopic cleat length, aperture, gas (purity 99.999%) is injected into the reference cell and then
and spacing were measured on pellets considering the connected to the sample cell at 77 K (−196 °C) under a liquid
microlithotypes (Table 6). nitrogen chamber. The adsorption and desorption isotherms
5.5. Spectroscopic Analysis (XRD). Identification of clay were obtained under relative pressures (P/Po) ranging from 0.05
and other coal minerals was carried out on sample size 150 μm to 0.99, where P is the balance pressure and Po is the saturation
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■ AUTHOR INFORMATION
Corresponding Author
Vinod Atmaram Mendhe − CSIR-Central Institute of Mining
and Fuel Research and AcSIR, Dhanbad 826015 Jharkhand,
India; orcid.org/0000-0003-3212-8298;
Email: vamendhe@gmail.com
Authors
John Buragohain − Department of Applied Geology, Indian
Institute of Technology (ISM), Dhanbad 826004 Jharkhand,
India; CSIR-Central Institute of Mining and Fuel Research
Figure 26. Relationship of physicomechanical properties with mineral/ and AcSIR, Dhanbad 826015 Jharkhand, India
clay content of coal samples. (a) Quartz content vs density. (b) Total Atul Kumar Varma − Department of Applied Geology, Indian
clay content vs density. (c) Quartz content vs compressive and tensile Institute of Technology (ISM), Dhanbad 826004 Jharkhand,
strength. (d) Total clay content vs compressive and tensile strength. (e) India
Quartz content vs Young’s modulus and Poisson’s ratio. (f) Total clay Priyanka Shukla − CSIR-Central Institute of Mining and Fuel
content vs Young’s modulus and Poisson’s ratio. Research and AcSIR, Dhanbad 826015 Jharkhand, India
Complete contact information is available at:
pressure.30,105,106 The Brunauer−Emmett−Teller equation https://pubs.acs.org/10.1021/acsomega.1c02041
(BET)79,107−109 was used to calculate the surface area as follows
C − 1 ijj P zzy
j z
WMC jjk P0 zz{
Notes
1 1
= + The authors declare no competing financial interest.
■
W ((P0/P) − 1) WMC
where W is the weight of the adsorbed gas at a relative pressure, ACKNOWLEDGMENTS
P/P0; Wm is the weight of the monolayer adsorbate; and C is a The authors are thankful to the Directors of IIT (ISM) and
constant related to the adsorption energy in the first adsorbed CSIR-CIMFR, Dhanbad, for granting permission to publish this
layer. paper. The authors are also grateful to Coal India, Ministry of
The surface area of samples completely covered by the Coal, Govt. of India, and M/s Oil and Natural Gas Corporation
nitrogen molecule monolayer is calculated using the equation St Ltd. for allowing the collection of coal samples from exploratory
1 C−1 boreholes and granting partial funding to support this research
= W M NA cs /M, where WM = slope + intercept , slope = W C ,
M work.
■
1
intercept = WMC
, N is the Avogadro constant (6.0221415 ×
1023 molecules/mol), M is the adsorbate molecular weight, and ABBREVIATIONS
Acs is the adsorbate molecules’ cross-sectional area. The results GSI Geological Survey of India
of surface area, pore volume, and pore size distribution are IS Bureau of Indian Standard
shown in Table 8. ASTM American Society for Testing and Material
5.7. Physicomechanical Properties. The coal core ISRM International Society of Rock Mechanics
samples were examined for different physicomechanical proper- ICCP International Committee for Coal and Organic
ties according to the methods suggested by the Bureau of Indian Petrology
Standards (BIS), i.e., the density and porosity110 (IS:13030), IUPAC International Union of Pure and Applied Chemistry
uniaxial compressive strength111 (IS:9143), tensile strength112 ICDD International Center for Diffraction Data
(IS:10082), Young’s modulus and Poisson’s ratio113 (IS:9221), ISO International Organization for Standardization
triaxial strength114 (IS:13047), point load strength115 (IS 8764), XRD X-ray diffraction
Protodyaknov strength index, and slake durability index116 SEM scanning electron microscope
(IS:10050) were determined. Also, refer to the Handbook of117 FE-SEM field emission scanning electron microscope
Brown, ISRM suggested methods for rock characterization, N2 nitrogen gas
testing & monitoring for the determination of uniaxial CO2 carbon dioxide
compressive strength, tensile strength, and other elastic SO2 sulfur dioxide
properties. The MTS 815, USA rock testing machine at CSIR- MCL master cleat
CIMFR, Dhanbad, was used (Table 9). FCL face cleat
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