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1. INTRODUCTION
To ascertain the potential uses of coal, several test are generally conducted. Some tests are physical
tests to determine how a coal behaves when it is being processed, for example, how difficult it is to
grind a coal. Other tests are designed specifically to determine whether a coal can be used to make
coke or whether it can be combusted, to name just two uses.
3. NON-DESTRUCTIVE TESTS
These tests are grouped as they do not change the core or sample in any way. They may disturb bore
core but it can be re-assembled afterwards into its original condition.
The information derived from the four tests described in this section can significantly assist the
geologist in establishing and confirming correlations and in subdividing the core for analysis.
These tests are usually applied to borecore, but may be used for any sample of uniform small cross-
sectional area.
5. CHEMICAL ANALYSES
5.1 Proximate Analysis
Proximate analysis is the most commonly used chemical analysis performed on coals. It is also the
simplest to perform. In this determination the inherent moisture, ash, volatile matter and fixed
carbon (by difference) are determined on a sample ground to pass 0.212 mm.
Moisture
A sample of about 5 gm is allowed to come into equilibrium with the laboratory atmosphere and
heated at 105C, in an inert nitrogen atmosphere, to constant mass.
The loss of mass is calculated as the moisture content.
This analysis is used to calculate the results of other analyses to a common (dry) basis. In any one
coal, oxidation will be indicated by an increase in moisture.
Ash
Coal ash, as distinct from mineral matter content, comprises the incombustible oxide residue
remaining after the coal has burned and all the volatile mineral constituents have been driven off.
In this analysis about 5 gm of coal is heated in air, under standard conditions, to 815C until
constant mass is achieved.
Volatile Matter
The volatile matter is determined from the loss of mass when about 5 gm of coal is heated out of
contact with air at 900C in a muffle furnace for 5 minutes. The result has to be adjusted for
moisture content.
This analysis measures not only the organic volatile matter content but also volatile constituents
evolved from the mineral matter such as carbon dioxide, water of hydration and sulphurous gases.
Fixed Carbon
Fixed Carbon is calculated using the formula: FC = 100 - (moisture + volatile matter + ash) all on
an air dried (a.d.) basis.
Like all coal tests and analyses it is usual to perform proximate analysis on duplicate samples and
the mean of the two analyses is taken as the result.
Nitrogen
The coal sample is decomposed catalytically with hot, concentrated sulphuric acid where the
nitrogen is converted to ammonium sulphate. Excess sodium hydroxide is added to liberate
ammonia, which is distilled and titrated against dilute sulphuric acid.
Sulphur
Sulphur occurs in coals as organic, sulphide or sulphate compounds. The sulphur determined as part
of an ultimate analysis is the total sulphur involving all these varieties.
The most commonly used method to determine total sulphur is the rapid high temperature method
where a coal sample is burned in oxygen at 1350°C where the sulphur is converted to gaseous
sulphur oxides. These oxides are absorbed in hydrogen peroxide to form sulphuric acid, which is in
turn titrated against sodium borate.
Oxygen
This is usually determined by difference.
Forms of Sulphur
If the sulphur, as determined during a total sulphur analysis, is high, say in excess of 1%, it may be
necessary to determine the forms in which the sulphur occurs, ie, organic, sulphate or sulphide.
High sulphur coals can lead to the following problems:
i. in steam-raising and domestic fuels the products of its combustion in the presence of water
form corrosive sulphuric acid;
ii. sulphur compounds can lower ash fusion temperatures and cause slag and foul the boiler
heating surfaces in power generation plants or domestic boilers;
iii. sulphur, mainly in pyritic form, in the presence of moisture is likely to promote spontaneous
combustion in coal stockpiles; and
iv. loss of plasticity in coking coals which result in increased coke consumption during iron
making operations, with associated higher slag volumes resulting in difficulty of furnace
control. High sulphur steels tend to be brittle.
The forms of sulphur are usually determined titrimetrically or calorimetrically.
Chlorine
Chlorine compounds can have the same corrosive effect on boilers as sulphur compounds so a
knowledge of the chlorine content of fuel coals is necessary.
Excess chlorine can cause a reduction in the softening and swelling capacity of coking coals, while
coals containing more than about 0.03% chlorine have a corrosive effect on refractory linings of
coke ovens unless made of silica.
Chlorine determination is usually carried out titrimetrically at the same time as the high temperature
sulphur analysis.
Phosphorous
All phosphorous in the washed coal enters the coke and it is considered, in Australia, that for iron
and steel making purposes a maximum of 0.05% in the washed coal is desirable. Phosphorous is
determined by spectrophotometry.
Mineral Matter
Determination of the mineral matter content of coals is necessary to convert, for comparison
purposes, coal matter properties such as carbon, hydrogen, volatile matter and specific energy to a
dry mineral matter free basis. The mineral matter content is always higher than the ash content and
is determined by completely oxidising the organic component of the coal sample in a
radiofrequency field applied to the analysis chamber containing oxygen at low pressure. This test is
not carried out frequently. However, recent developments of quantitative X-ray diffraction
mineralogical techniques may see this change in the near future
Ash Analysis
The ash of a coal contains the combustion residue of the mineral matter. The composition of the ash
is a useful guide to the minerals present in the coal when assessing the coal's slagging
characteristics in the blast furnace or on combustion
Normally the oxides of silica, aluminium, iron, calcium, magnesium, titanium, manganese and the
alkali metals are determined using one or more of the following techniques:
i. atomic absorption flame spectrophotometry; and/or
ii. x-ray fluorescence spectrometry; and/or
iii. optical emission spectrometry.
Apart from the major elements listed above other elements present in small amounts in a coal may
give rise to dangerous pollutants. A knowledge of the amounts of such trace elements as arsenic,
beryllium, cadmium, mercury and lead in coal-waste products is therefore desirable.
6. PHYSICAL TESTS
6.1 Specific Energy
The gross specific energy (also referred to as calorific value or heating value) is related to the actual
heat produced in a coal-fired boiler and is useful in comparing coals for this use. This property of
coal is obtained by ignition of a known mass of coal (usually 1 gm) in oxygen in a pressure vessel
surrounded by a water filled calorimeter. The gross specific energy is calculated from the
temperature rise of the water in the calorimeter and the mean effective heat capacity of the system.
The results are expressed as megajoules per kilogram (1MJ/kg = 430 btu/lb = 239 Kcal/kg).
The laboratory determination of specific energy takes place at constant volume while industrial
combustion takes place at constant pressure. For coal, the difference between gross specific energy
at constant pressure and that at constant volume is not significant.
In industrial practice, the gross specific energy is not achieved as the water vapour in the
combustion products cannot be condensed. The following formula allows calculation of the nett
specific energy.
Qnettas = Q grossas - 0.0245 (Mas + 9Has)
where:
Qnettas = nett specific energy as sampled in MJ/kg.
Q grossas = gross specific energy as sampled in MJ/kg
Mas = total moisture as sampled in %
Has = hydrogen as sampled in %
Australian practice regards coals for power generation purposes with a gross specific energy of
more than 26 MJ/kg as satisfactory, while high quality coals will have values exceeding 30 MJ/kg.
The Hoehnepalstometer, used in parts of Western Europe, produces higher maximum fluidity
values than the Gieseler plastometer.
Precision values are:
Maximum fluidity (log10) 0.10
Characteristic temperatures (°C) 5
(b) Koppers Swelling Test. This test produces information on the swelling characteristics of coal
and in particular is used to predict the pressure applied to the walls of a coke oven during the
coking process.
(c) Penetration Plastometer. This test is little used in borecore evaluation because it requires a
relatively large sample mass. Correlations can be made between results of this test and laboratory
coke oven tests.
(d) Small Scale Coke Oven Tests. The most desirable method of assessing the coking potential
of a single coal, or blend of coals, is to perform small scale coke oven tests. The advantage of this
technique is that it produces coke samples than can be subjected to physical property measurements
as well as chemical and strength tests.
In general large pilot coke ovens (100 kg or more) are preferred, because these ovens can more
reliably simulate commercial practice, but smaller ovens of 7 kg and 15 kg capacity have been
developed to accept the smaller sample sizes that are often available from the concluding phases of
an exploration programme.
(e) Gray-King Carbonisation Assay. This test measures the yields of gases, tar, liquor and coke
on carbonising a small sample of coal at 600°C (low-temperature assay) or about 900°C (high-
temperature assay). In addition, the coke is examined and its nature ranging in type from
pulverulent through coherent to very highly swollen is reported. The results of this assay
complement that obtained from proximate and ultimate analyses. Different coals with the same
analyses can give different results in the Gray-King assay.
In the test a 20 gm sample of air-dried coal, ground to pass 0.212 mm is heated in a fused silica tube
to 300°C to expel expanded air and gas, then at a uniform rate to 600°C (900°C) in l h (2 h), and
held at the fmal temperature for l h (30 min). The products of decomposition are cooled, liquids
condensed, ammonia absorbed in dilute acid and the gas collected and its volume measured. If
required, the gas can be analysed to determine its composition and heating value after correcting for
water vapour and initial air in the system.
The yields of all products and coke (after cooling) are determined. The coke is visually examined
and compared with photographs of standard coke types given in the published method.
The test indicates the likely relative product yields and distribution as well as the caking
behaviour of the coal in large-scale carbonisation operations. However, it must be noted that the
yield data in this test rarely coincide exactly with large-scale yields of pyrolysis which depend
heavily on process conditions such as heating rate and residence time of volatile products.
(f) Fischer Carbonisation Assay. This test determines the yields of tar, water, gas and coke
residue by low temperature distillation of brown coal and lignite, and forms the basis for the
classification of brown coal and lignite for use in low temperature carbonisation.
The test is also used in the evaluation of oil shales.
In one method, the sample is heated in an aluminium retort to 520°C during a period of 80
minutes. The products of decomposition pass into a water-cooled receiver; the tar and water are
condensed while gaseous products pass to the atmosphere. The coke residue remaining in the
retort is weighed. The receiver and its contents are also weighed and the mass of the water in the
receiver determined by entrainment with toluene or xylene: the mass of tar is obtained by
difference. The total water in the receiver includes the moisture in the coal as well as that from
the decomposition of the coal. A separate determination of moisture in the coal, also by
entrainment with toluene or xylene, is made so that the decomposition water can be calculated.
The percentage of gas (plus errors) is obtained by subtracting from 100 the sum of the percentage
of coke residue, of tar and of decomposition water. The results are reported on the 'as analysed'
and on the 'dry' basis.