ter 3

LABORATORY METHODS
5.1 PREPARATION OF COAL SAMPLES

5.1.1 Powdered samples

The samples of coal collected from the field are air dried to

remove the free moisture. After drying, the required amount (250 gm)

is taken from each sample by coning and quartering method. The

portion selected is crushed and passed through 72 mesh (211 micron)

sieve. Powdered samples are collected and stored in air tight glass

bottles and these samples are used for chemical analyses in the

laboratory.
Chapter 5 44

5.1.2 Polished blocks

Polished blocks are prepared from the channel samples

selecting hard lumps of coal. In order to prepare polish blocks to

study the coal under reflected light, tw,o alternate faces (vertical and

horizontal) are selected. The faces are then ground by increasing fine

grades of carborandum powder upto 600 grade on a revolving disc in

wet condition. The blocks are then polished on a plane glass using

y-alumina suspension. Then block is washed with water to remove

impurities. The washed surfaces are polished by using emery papers

from 004-001 grades.

Final polishing is made in a sylvet cloth fitted on a revolving

disc.

5.2 DETERMINATION OF SPECIFIC GRAVITY

The specific gravity of the samples is determined by using

specific gravity bottle (pycnometer) taking teepol solution as the

medium.

5.3 CHEMICAL ANALYSES OF COAL

5.3.1 Proximate analysis

The proximate analysis of coal includes the determination of

moisture, volatile matter, ash, fixed carbon and calorific value. The

first three are determined in laboratory and the fixed carbon is found

out by difference The calorific value is calculated with the help of the
Chapter 5 45

proximate analysis data using Goutal’s formula, The proximate

analysis is carried out by adopting the procedures as recommended in
-Indian Standard-Methods of Test for Coal and Coke (I.S.I., 1981).

5.3.1.1 Determination of moisture

Moisture in coal may be present as adsorbed water on external

surface of coal or in the capillary of pores present in the coal and this
is termed as free or accidental moisture. It is also present as
combined water, as water of hydration of inorganic constituents, as
dissolved water resulting from decomposition of organic compound
and this is distinguished as inherent or hygroscopic moisture. The
free moisture can be removed by air-drying but the inherent moisture
can only be removed completely by drying in an oven at 100+5°C for
about an hour. The added amount of free and inherent moisture is
called total moisture.
A moisture capsule consisting of two shallow glass dishes is
cleaned and dried. The weight of the capsule is taken and one gram
of coal is weighed in the capsule (wi). Coal is spread with a brush in
one dish. Then it is heated in an electric oven out of contact with air
(to avoid oxidation) at 100+5°C temperature for an hour.
After heating, the capsule is transferred to a desiccator and
rapidly reweighed (W2 ). The difference in weight (i.e., wi - W2 ) will
give the amount of moisture. Moisture content is expressed in per
cent of coal.
Chapter 5 46

5.3.1.2 Determination of ash content

The residue left after burning of coal is known as ash. It is

generally composed of inorganic substances.
1 gm of coal is weighed in a silica basin (wi). Coal is spread
with a brush. Then the basin is kept inside a muffle furnace and the
temperature is gradually raised upto 800°C. At 800°C the
temperature is kept constant and the incineration of coal is completed
by heating the coal for an hour at that temperature. After incineration,
the basin is allowed to cool and transferred to a desiccator. After
sometime the basin is re-weighed (W2 ). Deduction of wi (weight of
the basin) from W2 (weight of the basin + ash) gives the amount of ash
in the coal. Ash content is expressed in per cent of coal.

5.3.1.3 Determination of volatile matter

The volatile matter, sometimes called volatiles consists mainly

of the gases and water and tarry vapours evolved from coal when it is
heated at high temperature.
To determine it, 1 gm of coal is taken in a silica crucible with a
porous silica cover. The weight of the silica crucible and coal is wi.
The cover is used to avoid oxidation. The coal is then heated for 7
minutes at a constant temperature of 925°C inside a furnace. After
heating the crucible is cooled and transferred to a desiccator. After
few minutes the silica crucible is re-weighed (W2). The difference
between wt and w2 gives the amount of apparent volatile matter in the
Chapter 5 47

coal. The actual volatile matter is obtained after deducting the

moisture content of the sample. Volatile matter content is expressed
in per cent of coal.

5.3.1.4 Calculation of fixed carbon (F.C.)

The fixed carbon represents the carbon content in a coal that

has not combined with any other element (in a free state). The
amount of fixed carbon increases with the rank of coal and is highest
in Antracite coal.
The amount of fixed carbon is computed by subtracting the sum
of the percentage of moisture, volatile matter and ash from hundred.

Fixed carbon = 100 - (moisture% + ash% + volatile matter%)

5.3.1.5 Calculation of mineral matter (M.M.)

The mineral matter in coal represents the inorganic mineral present in

it. It is left as residue or ash after complete combustion of coal or
coke. The residue is made up of non-combustible mineral matter
consisting of silicates of calcium, magnesium, iron and titanium,
oxides of iron and silicon, carbonates of iron, calcium and magnesium,
sulphate of calcium and some phosphates.
The actual amount of mineral matter in coal is calculated using
the following formula :
Mineral matter = 1.08 x ash + 0.55 x pyritic sulphur
Chapter 5 48

5.3.1.6 Fuel ratio

It is the ratio between fixed carbon and volatile matter

(F.C./V.M.). In early classification of coal it was used as one of the
parameters for classification.

5.3.2 Ultimate analysis

The ultimate analysis of coal involves the estimation of carbon,

hydrogen, nitrogen, sulphur and oxygen. The first four elements are
determined directly but as there is no satisfactory method for the
direct determination of oxygen in coal, the amount of oxygen is found
out by difference.

5.3.2.1 Determination of carbon and hydrogen

Carbon and hydrogen are determined simultaneously by the

combustion tube method as described in Indian Standard Methods of
Test for Coal and Coke (ISI, 1974). The coal sample is burnt in a
current of oxygen-AII the hydrogen is converted into water and all the
carbon to carbon dioxide. The products are absorbed by suitable
reagents and determined gravimetrically. The oxides of sulphur are
retained by lead chromate, chlorine by silver gauze and oxides of
nitrogen by red lead.
Chapter 5 49

5.3.2.2 Determination of nitrogen

The nitrogen content in coal is determined digesting coal

sample (1 gm) in Kjeldahl flask with potassium sulphate, selenium
oxide and sulphuric acid and subsequently by distillation and titration.

5.3.2.3 Computation of oxygen

As there is no satisfactory method for the direct determination

of oxygen, it is calculated by difference, that is, sum total of carbon,
hydrogen, nitrogen and organic sulphur and deducted from 100 is
taken as oxygen or oxygen % = 100 - (C% + H% + N% + organic
sulphur %).

5.3.2.4 Determination of total sulphur

The total sulphur content of coal is determined gravimetrically

by Eschka method.
In this method, powdered coal sample is heated in intimate
contact with Eschka mixture (two parts of calcined magnesia and one
part of anhydrous sodium carbonate by weight) in an oxidising
atmosphere to remove combustible matter and to convert all forms of
sulphur to sulphate. This is then extracted and determined by
gravimetric method by precipitation as barium sulphate with barium
chloride.
Chapter 5 50

5.3.2.5 Determination of forms of sulphur

Sulphur is usually present in coal in three forms - as sulphates,

as iron pyrites (FeS2) and as sulphur in organic compounds. The

forms of sulphur so present are known as ‘sulphate’, ‘pyritic’ and

‘organic’ respectively.

Sulphate sulphur is determined by extracting coal with dilute

hydrochloric acid and determined gravimetrically by precipitation as

barium sulphate with barium chloride.

Pyritic sulphur is insoluble in dilute hydrochloric acid, but is

quantitatively dissolved by nitric acid under experimental conditions

and converted into sulphate. The sulphates are separated from nitric

acid by evaporating nitric acid. The sulphates are extracted with

hydrochloric acid and determined gravimetrically by precipitation as

barium sulphate with barium chloride.

Organic sulphur of coal is not determined by analytical method,

it is calculated by deducting the sum of pyritic and sulphate sulphur

from total sulphur.

5.3.3 Determination of the calorific value by Bomb Calorimeter

The calorific value of Bapung coal is determined in the

laboratory with a bomb calorimeter [IS : 1350 (part - II - 1970)]. 1

gram of coal is burnt in an atmosphere of oxygen under a pressure of

about 25 atmosphere. The coal inside the bomb is ignited electrically.

The bomb is placed in 0.5 cc water. The heat produced is absorbed

C hapter 5 51

in the water. The rise in temperature of the water after the

combustion is measured with a Beckmann thermometer.

5.3.4 Calculation of calorific value

The calorific value of the Bapung coal is also calculated from

proximate analysis data using the Goutal's formula as given below

P = 82 C + cxv

where, P = the number of calories in a gram of coal

C = the percentage weight of fixed carbon on air dried

coal

V = the percentage weight of volatile matter on air dried

coal

a is the constant which varies oppositely to the volatile

matter (v?) estimated on a dry mineral matter free basis,
which can be readily read off from a chart prepared for
that purpose (Moore, 1950).

5.3.5 Calculation of useful heat value

The useful heat value of coal is defined by the following formula

HU = 8 9 0 0 - 138 (A+M)

Where, HU = useful heat value in calories per gram

A = The percentage weight of ash on air dried coal
M = The percentage weight of moisture on air dried
coal

The above formula is used for calculating useful heat values of

Gondwana coal having high ash content. The coal deposits of North

East India is having comparatively lower percentage of ash than the

Gondwana coal. The formula modified for the coal deposits of this

region is as follows (Phukan et al., 1998).

Chapter 5 52

HU = 8000 - 138 (A+M)

The above formula for calculation of useful heat value of Bapung

coal is used.

5.4 LOW TEMPERATURE CARBONISATION

The low temperature carbonisation of coal is done at a

temperature of 600°C to determine the coke, tar, liquor and gas yield

of the coal. In the experiment 20 gram of coal is kept in a silica retort

with an asbestos plug and the silica retort is inserted into the hot

furnace. The retort is connected with a receiver to collect tar and

liquid products of carbonisation. The receiver is kept in an ice bath to

cool the vapours coming out of the silica retort. It is connected to a

gas collecting bottle filled with water. The pressure inside the gas

collecting bottle is always kept equal to the atmospheric pressure.

Gases released from the silica retort during carbonisation are

collected in the bottle replacing water. After keeping coals in the

retort and fitting every apparatus properly, the temperature of the

furnace is steadily increased at a rate of 5°C/minute to a constant

temperature of 600°C and this temperature is kept for one hour. The

gases separated are collected in the gas collecting bottle, tars are

collected in the receiver and cokes are left in silica retort. The nature

of coke is determined by correlating it with some photographs of some

standard types.
Chapter 5 53

5.5 DETERMINATION OF TRACE ELEMENTS IN COAL

The trace element contents of coal are measured by using the

Perkin Elmer Atomic Absorption Spectrometer (model - 3110). For

this purpose 2mg of each coal samples are burnt at 700°C for an hour

to obtain ash. The ash of the samples are digested in a mixture of 5

ml HF, 4 ml HNO3 and 0,5 ml HCIO4 in teflon bomb for one hour at

140°C. After that the mixture is mixed with H3 BO4 solution (5 ml

H3 BO4 in 40 ml of water), filtered and the volume of the solution is

made upto 100 ml. These solutions are used for elemental analysis.

The analysed trace elements are Pb, Cu, Ni, Mn, Zn, Co, Cr.

5.6 DETERMINATION OF MICROHARDNESS OF VITRINITE

From the polish surfaces the Vicker’s microhardness of vitrinite

(perpendicular to bedding plane) is determined with Mini Load

Hardness Tester. For an exact determination of the hardness, care is

taken such that the impression of the diamond pyramid is situated in a

zone of the maceral which is free of fracture and mineral impurities.

The polished sample is placed in the mechanical stage of the

hardness tester. The area measured is selected with the objective

with magnification 10. To check the homogeneity of the area chosen,

the 40x measuring objective is brought into position by means of a

rotating objective changer. Then the measuring objective is moved

out and the diamond pyramid placed in position. A load of 100 g is

applied to the pyramid. By means of a trigger a spring is released

Chapter 5 54

which allows the diamond to penetrate into the surface of the vitrinite.

The time during which the load is applied can be regulated by an oil

‘brake’; it should always be 15 seconds. After a total time of 30

seconds has elapsed from the beginning of the operation, the

diamond is lifted and swivelled back; the measuring objective is then

placed in position. The two diagonals of the impression are measured

with the precision eyepiece, the Vicker’s hardness being calculated

from the formula (Stach et at., 1982)

1854.4P
HVkp/mm2

Where, P = 100g
d = length of the diagonals in microns.

5.7 DETERMINATION OF pH, CONDUCTIVITY, TOTAL DISSOLVED

SOLID (TDS) OF MINE WATER

5.7.1 pH

The pH of mine water is determined by using WTW, ‘MERCK’

Germany make portable pH meter (model pH 320).

5.7.2 Conductivity

The conductivity of mine water is measured by using WTW, ’MERCK’

Germany make portable conductivity meter (model LF 320).

5.7.3 TDS

The TDS is also measured in the laboratory by using WTW,

'MERCK' Germany make portable equipment (model LF 320).