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3.

METHODOLOGY

3.1

VISUAL MACERAL ANALYSIS

3.1.1 REFLECTED LIGHT TECHNIQUE


The reflected light technique requires that the coal sample be optically
polished and free of scratches. The samples are studied with the aid of an
incident light microscope using either oil immersion or dry objectives. The
incident light technique enables one to observe a sharp, detailed image of
the coal.
The resolution of polished surface, particularly in oil immersion, is much
better than in the thin section technique, the quantitative count of
macerals is more accurate and the ability to measure the reflectance of
the macerals is enhanced. Polished sections are better observed at 40 to
60 magnifications.

3.1.1.1

PREPARATION OF POLISHED SECTIONS

Polished Blocks
Blocks of coals of suitable size are usually cut from a column sample of a
coal bed. Individual blocks are clearly labelled as to their stratigraphic
position and orientation in the coal bed. If the blocks are highly fractured,
embedding in an epoxy resin may be necessary prior to cutting into
smaller blocks. A block with cross-sectional surface area about 5 x 10 cm
is usually adequate for such preparation and is primarily prepared for
macroscopic examination. For microscopic investigation the blocks should
be cut small enough such that they will fit into cylindrical molds 2.54 cm
(1 in.) or 3.18 cm (1.25 in.) in diameter, filled with epoxy, cured and
polished with automated grinders and polishers.
Polished Briquets
Polished

briquets

(pellets)

are

made

from

crushed

coal

samples

representing an entire coal bed or blend of coal samples. Coal sample is


first crushed with a suitable crusher such as a roll mill so that all coal will
pass through a standard 4-mesh screen, with minimum fines generated.

The crushed coal is then further crushed with a hand mill or a power mill
that revolves at 30 rpm or less. The throughput is sieved with a 20-mesh
(850 m) screen. The oversize material is crushed and sieved again until
all of it passes through the 20-mesh screen. Five to six stages of crushing
may be required in order to generate the minimum amounts of fines (less
than 40 m). The crushed coal is then mixed with an epoxy resint mixture
in the ratio of about four parts coal to one part epoxy by volume,
thoroughly mixed and filled into a cylindrical steel mold 2.54 cm (1 in.) or
3.18 cm (1.25 in.) in diameter. The coal-epoxy mixture is then briquetted
under a pressure of approximately 350 kg/cm2 (5000 psi) for 2 min. a
releasing agent must be used to avoid bonding the briquette to the mold.
The briquette is then allowed to cure in the mold overnight. After removal
from the mold, the briquettes are placed in a holder and are ready for
grinding and polishing with an automated grinder/polisher. The briquettes
are ground successively with 240, 400 and 600 grit silicon carbide paper
and 5.0 and 0.3 m alumina on synthetic cloth and 0.05 m alumina on
silk.

3.1.2 TRANSMITTED LIGHT TECHNIQUE / THIN SECTION TECHNIQUE


The thin section techniques requires that the coal be cut or ground into
thin sections on the order of 10 m thick and studied under transmitted
light. The transmitted light technique covers a larger area in a single field
of observation, thus providing a larger picture of the samples examined.
Thin sections of coal exhibit brilliant colour ranging from yellow to orange,
red and brown to opaque that illustrates well the individual macerals
grains, grain size, orientation and relationship with other macerals and
minerals. In most cases thin sections are made in an orientation
perpendicular to the bedding planes so that the intergranular relationship
is well preserved. Thin sections are usually examined with a low power
(x10) objectives for best results.

3.1.2.1

PREPARATION OF THIN SECTIONS

To view coal in transmitted light, it must be ground to a thickness of about


10 m. Coal is relatively soft material and to grind it to a thickness of 10
m requires extreme care to ensure a good result. Thus, coal thin sections
are usually done by hand, with some help by automated grinding
equipment.
First a block of coal about 2 x 4 cm in cross section is cut with the short
dimension perpendicular to the bedding plane. This surface is then ground
with 240, 400 and 600 grit silicon carbide wheel or paper disk.

A flat

surface must be maintained at all times. The surface is then ground on a


Belgian hone, made of a Belgian lithographic limestone.
The direction of grinding on the hone is parallel to the bedding plane of
the coal so that any fine scratches made on the hone will be parallel to the
bedding plane. After cleaning this surface with acetone, it is dried and
bonded to a 2.5 x 7.6 cm (1 x 3 in.) glass slide with epoxy resin. After
curing, the excess coal is cut with a fine cutting saw, leaving a thin slab of
coal about 1-2 mm in thickness. The excess coal is then ground with 240,
400 and 600 grit grinding wheels or paper disks until megaspores or
cuticles appear red when the slide is viewed in front of a light source. The
remaining grinding is done on a Belgian hone until a uniform and desirable
thickness is reached. The slide should be examined periodically under a
transmitted light microscope. The thin section is considered finished when,
in the case of high volatile bituminous coals, liptinite appears to be
brilliant yellow and vitrinite vivid red. A cover glass is placed over the coal
thin section using Canadian balsam as the mounting medium.

3.2

VISUAL KEROGEN ANALYSIS

3.2.1 PREPARATION OF SAMPLES


There are 4 steps for extraction process. Firstly, dry samples are crushed
to less than 32 mesh size with iron mortar and pestle. Next, the sediments
will be placed into a beaker and dissolved in 5 N HCL, followed by 10 N
HCL and 46% HF (1:1) for three times. This is to remove any carbonates
and eliminate most of the non-calcareous minerals debris from the
residue. Thus leaving behind will be the organic material known as

kerogen. The organic matter is separated

from the remaining mineral

debris and concentrated by flotation in a heavy liquid (zinc bromide).


Undissolved kerogen samples will be washed with distilled water using
centrifugation until neutral. The separated kerogen samples will be placed
on a non-flourescent slide glass with a small amount of Entellen neu
(Merck), then covered with a micro cover glass. The kerogen will be
observed on a light fluorescence microscope.

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