2 Chemical Analysis and Classification of Coal

2 Chemical analysis and classification of coal
2.1 INTRODUCTION
Coal is a heterogeneous mixture of organic compounds,
together with a certain amount of inorganic material in the
form of moisture and mineral impurities. The nature of the
organic constituents depends on the relative proportions of
the various kinds of plant debris (wood, leaves, spores etc.)
in the initial accumulation of peat (the coal type), and on the
diagenetic or metamorphic changes that have occurred since
the peat was originally laid down (the rank of the coal).
Together with the nature and relative amount of any mineral
matter that may be present, this assemblage of organic
compounds is reflected by the physical appearance of the
coal, and determines its behaviour when used.
2.1.1
Classes of coal analysis
An account of the various organic compounds actually

present in coal is given by Francis (1961), van Krevelan
(1961) and Flaig (1968). This type of analysis is only
attempted as part of a detailed research investigation. For
most practical purposes, the general nature of these materials
can be evaluated by a combination of two sets of analytical
data:
(a)
Proximate analysis
This gives the relative amounts of light organic compounds

(volatile matter), as opposed to non-volatile organic material
(fixed carbon). This type of analysis also gives the amount
of moisture in the coal, and a measure of the inorganic
components, left as a residue or ash when the coal is burned.
(b)
Ultimate analysis
This determines the total amounts of each of the principal

chemical elements in the coal: carbon; hydrogen; oxygen;
nitrogen and sulphur. In some studies, the data may be
recalculated to remove the percentage of these elements
contained in the moisture and mineral impurities, in order to
obtain the chemical composition of the organic fraction
alone.
In many cases, the results of proximate and ultimate
analysis are sufficient to indicate how the coal will behave in
industrial use. More specific tests may also be employed to
give further information on various aspects of the coals
properties. These tests may be regarded as miscellaneous

analyses, and include determination of such properties as
the amount of heat energy liberated from the coal on
combustion, and the type of coke likely to be made from the
coal in carbonization processes. Other mechanical
properties, such as the coals relative density, and its
amenability to upgrading in preparation plants may also be
investigated.
2.1.2
Errors in analysis
The methods of sample collection and laboratory testing for

coal analysis have been refined by the experience of
numerous workers in the field, and standardized procedures
have been drawn up to minimize the likelihood of error.
Most of the tests are covered by various national or
international standards (Appendix 1), and, in commercial
evaluations, strict adherence to these procedures is generally
necessary. However, as many of the national standards for
the same test may differ in points of detail, it is also
necessary to indicate, when stating the results, which
particular method was followed.
Errors in analysis may arise from a number of sources
including sample collection, sample storage, and the actual
performance of the testing operation. In some cases, such as
with errors introduced by biased sampling procedures or
incorrectly calibrated laboratory instruments, they may not
be immediately apparent, and the erroneous results
incorporated, without question, into a far-reaching quality
assessment.
Many of the laboratory techniques in coal testing are
based on arbitrarily chosen dimensions, materials,
temperatures and heating rates, and errors may also be
introduced if these procedures are not followed exactly. In
other cases, however, the coal itself may be oxidized, or
contain components that give rise to unusual test results.
Rees (1966) gives a very complete discussion of the sources
of error that may arise in a number of the tests commonly
performed.
2.2
SAMPLING FOR COAL ANALYSIS
Even the most precise analytical determination is useless for

most practical purposes if the sample tested does not truly
represent the mass of coal from which it was taken. Coal
samples may be taken from outcrops, mine faces and other
in situ exposures, from
Chapter 2
drill cores or cuttings, and from masses of broken coal such

as in conveyor belts and stockpiles. The procedure for
collection of these samples is also covered by many national
standards, and these should be followed in detail if bias is to
be minimized.
2.2.1
Sampling a coal face
An in situ exposure of a coal seam in a mine or outcrop is

normally sampled along a line running perpendicular to the
bedding planes. The sample may be taken by one of the
following methods:
(a) Pillar sampling
This involves taking a continuous rectangular block of coal,
extending between the upper and lower bedding planes
marking the limits of the interval in question. The block is
normally 30-45 cm wide and around 450 cm2 in cross
sectional area. Pillar samples are very time consuming (and
therefore costly) to obtain, as well as difficult to handle, and
are seldom used except for detailed research work.
(b) Strip or channel sampling

This involves cutting a channel or groove into the coal face,
and collecting all of the pieces removed on a clean plastic
sheet at the base of the exposure. The channel should have a
cross sectional area of at least 100 cm 2, and sufficient
material taken to give around 15 kg of coal per metre of
seam thickness.
For bulk sampling in well-known seams, the pillar or
strip sample may extend, without break, from the roof to the
floor of the interval in question. However, where significant
partings, or bands of non-coal material occur (Section 5.2.1),
the sample may be divided into sub-sections or plies
between these natural breaks (Fig. 2.1).
The amount of material in these strip or channel samples
may be reduced, if necessary, by the cone and quarter
technique to give a more suitable mass for transport.
Samples from which it is intended to determine the total
moisture content (i.e. before air-drying; Section 2.3.2)
should be sealed in dry, airtight containers immediately after
the sample is collected.
2.2.2
Sampling coal by drilling
The methods used in exploratory drilling of coal seams are

described more fully in Section 6.5. Due
to the risk of contamination, samples of cuttings from noncored holes are of limited value for coal analysis. However,
because they are obtained easily and at low cost, they are
sometimes used for the rapid appraisal of certain aspects of
seam quality, such as the extent of oxidation in the outcrop
zone. The rank of the coal may also be assessed by
petrographic examination of material taken from the cuttings
of non cored holes (Section 3.6).
Cores samples of the coal seams are required for more
comprehensive analytical programmes. Selection of the core
size to be used depends partly on the anticipated drilling
conditions, and partly on the amount of material needed to
perform all the necessary tests on the thickness of coal
involved. Small diameter (20 mm) cores tend to give less
complete seam recoveries in banded or friable coals, and
cores of around 45-60 mm diameter are more suitable for
most studies. Large- diameter cores, up to 200 mm in
diameter, are needed to provide samples for detailed
washability tests (Section 8.2.7).
A core sample of a coal seam is equivalent to a pillar
sample with a small cross-sectional area, and can readily be
divided into plies or sub-sections for analysis. Special
attention may need to be given to cores where recovery of
some segments of the seam is incomplete. Care should be
taken in these cases to ensure that the mass of material from
each segment included in the analysed sample is in
proportion to its mass (length x relative density) in the total
ply being studied. The need for these reconstructions in the
sampling operation can be judged from details of the core
recovery, measured either on a linear or, preferably, a
volumetric basis.
2.2.3
Sampling of broken coal
Fig. 2.1 Channel sample collection from a coal seam on a ply-by-ply basis.
Chemical Analysis and Classification of Coal
Coal from
v. stacker
Fig. 2.2 Segregation of particles in a simple stockpile.
In a mass of broken coal, such as a stockpile, the particles

tend to become segregated, with denser orfiner particles
occupying different positions to the coarser or lighter
components (Fig. 2.2). Sampling procedures in such cases
must take this segregation into account in order to avoid the
introduction of a bias to the subsequent analytical
programme. The sampling operation may be covered by a
national standard or other set of similar guidelines, and these
should be followed rigorously to ensure good results. The
mass of material taken depends partly on the requirements of
the tests to be performed, and partly on the physical size of
the coal fragments involved.
2.2.4
Sample preparation
Once transported to the laboratory, the methods of sample

preparation depend on the nature of the material and the
analyses or tests to be carried out. Although the most
effective procedures are best determined for each individual
analytical programme, some typical requirements are:
(a) Broken coal
Where the total moisture content is to be determined
(Section 2.3.1), the sample must be transferred to the
laboratory in an air-tight container. The mass of the
wet coal is determined on arrival, after which the coal is airdried and reweighed prior to further testing. If necessary, the
particle size distribution is also determined on the air-dry
coal. Appropriate size fractions may be split off and
subjected to float-sink or other washability tests if necessary
(Section 2.6.3), prior to crushing for analysis (Fig. 2.3).
(b) Exploration cores
Chapter 2
The core is generally transported to the laboratory with as

little disturbance as possible. It may then be subjected to
non-destructive tests such as X-radiography (Section 6.5.7),
or ply-by-ply relative density determination (Section 2.6.1)
as well as detailed
Bulk sample from

stockpile etc.
Transport in
sealed container
Determine total
moisture or air-dry
moisture loss
Determine particle size

distribution
--------1
Fine fraction
Coarse fraction(s)
Crush and analyse

Reserve
\
Float-sink testing Froth flotation testing
Each density fraction
r---------------------) i
Crush and analyse

Reserve
Product and tailings
Crush and analyse [ Combine as required to form

Reserve
I
Crush and analyse
Reserve
11.
Reconstituted clean-coal products Reconstituted refuse materials

Further testing and analysis Further testing and analysis
Fig. 2.3 Possible laboratory preparation flowsheet for a broken coal sample.

macroscopic logging (Section 3.2.3). The seam is divided
into sub-sections for analysis, if necessary, after the
volumetric recovery of each significant interval has been
determined.
Where washability testing of slim cores is required, the
plies to be treated separately are crushed to a nominated top
size (usually between 10 and 15 mm) in a way that produces
a minimum proportion of fine particles. Large-diameter
cores may be subjected to a special crushing and tumbling
technique to simulate the effects of particle size reduction
and degradation by the mining and handling process
(Section 8.2.3). In both cases, splits can also be riffled off for
analysis of in situ (i.e. raw) coal properties, but the major
part of the material is subjected to float-sink or similar
testing (Fig. 2.4), before being more finely crushed for
detailed studies of the clean coal products.
Almost all analysis requires the coal to be air-dried.

After crushing, the sample is spread out and allowed to dry,
without heating, in either the laboratory atmosphere or a
humidity-controlled drying cabinet. The analytical results
are initiallycalculated in relation to the air-dried coal,
although they can also be re-expressed to any other basis
(e.g. dry, ash free) if necessary (Section 2.10.1).
2.3
PROXIMATE ANALYSIS
As indicated in Section 2.1, proximate analysis gives a

measure of the relative amount of volatile and non-volatile
organic compounds in the coal as well as the percentage of
water and non-combustible mineral materials. If corrections
are applied to compensate for the non-organic impurities,
proximate analysis enables the organic component of one
coal to be compared with that of another, and hence provides
much of the basic data for systematic coal classification. In
commercial applications, however, it is normal for the coals
properties to be assessed with all of the impurities included,
as this represents the actual product that is to be used.
f------Each coal ply
Coarse crush
Fine crush
and analyse
Fine crush
and analyse
'
Reserve
Combine with other

coal plies to form
working section coal
composite
Combine with other noncoal plies to form

working section noncoal composite
---------)
Each non-coal ply
Coarse crush
1
Reserve
f----------
Float-sink testing
Each density
fraction
Bore core
X-radiography Detailed logging

Density and recovery determination
I____________________
H---------------------)
Combine with appropriate other fractions to form Reserve

I
- Shale breakdown testing
Fine crush
and
analyse
Chapter 2
Reconstituted clean-coal product
Further testing and analysis
Reconstituted refuse material
Further testing and analysis
Fig. 2.4 Possible laboratory preparation flowsheet for an exploration bore core. Other procedures may be followed as well, depending on the
sample and the data required. (Modified from Australian Standard 2519, 1981.)
2.3.1
Moisture
The moisture in a coal may occur in four possible forms:

(a)
Surface moisture
This is extraneous water held as films on the surface of the

coal particles.
(b) Hygroscopic moisture
This is water held inside the capillaries of the coal substance.
(c)
Decomposition moisture
This is water incorporated in some of the coals organic

compounds.
(d) Mineral moisture
This is water which forms part of the crystal structure of
clays and other minerals present in the coal.
A coal sample collected from a mine or stockpile is
usually wet with a variable amount of adventitious
moisture from seepage, water sprays, rain and other sources.
Such water is surface water, and generally evaporates readily
in the laboratory atmosphere. The amount of mositure in
other forms, often regarded as inherent moisture, is more
or less constant for coals of a given rank. Much of it,
especially the moisture in the pores of the coal, is driven off
by heating to 100 C, but some of the mineral and
decomposition moisture may not be liberated until
temperatures exceed 500 C.
A coal that is sold commerically usually contains a
certain amount of surface water, and the mass of this water is
naturally included in the mass of coal that is delivered.
Knowledge of the total moisture content of the coal (i.e.
adventitious + inherent moisture) is therefore essential to
assess the value of any marketable consignment. However,
because the amount of surface water is difficult to control,
separate assessment of inherent or air-dried moisture is also
necessary, as most other analyses are carried out on air-dried
material.
(a) Total moisture
Determination of total moisture is based on the loss in mass
between the sealed sample as received in the laboratory
(Section 2.2.4) and that of the same sample fully dried. The
moisture is driven off by one of the following methods:
(i) Distillation with toluene the coal is heated under
reflux with toluene and the mass of water collected as a
condensate is determined.
(ii) Drying in a minimum free-space oven the coal is
dried at 105-110C in an atmosphere of flowing nitrogen in a
small, specially designed oven and the relative loss of mass
is determined.
(iii) Oven-drying in air the coal is dried at 105
110C in a laboratory air oven and the relative loss of mass
is determined.
Methods (i) and (ii) are suitable for total moisture
determination in coal of all ranks, but because of the
possibility of oxidation in low-rank coals, method (iii) is
normally used only with high-rank materials. High-rank
coals may also be air-dried before the final drying process,
enabling the air-dry loss or free moisture content to be
determined separately.
(b) Inherent or air-dried moisture
The inherent or air-dried moisture content is represented by
the relative loss of mass when the air-dried coal is heated,
without oxidation, to a little over 100 C. It may be
determined by one of the following techniques:
(i) Drying in a minimum free-space oven the coal is
dried at 105-110 C in a special small oven with a flowing
nitrogen atmosphere, and the relative loss of mass
determined.
(ii) Direct gravimetric determination the coal is sealed
in an atmosphere of dry nitrogen, heated to 105-110 C and
the water collected in an absorption tube. The relative mass
of water collected gives the moisture content of the coal.
(iii) Drying in vacuo the relative loss of mass is
determined when the coal is held at 105-110 C for a
specified time under a vacuum of less than 5 mm Hg.
Because of its capacity to treat a number of samples
simultaneously, use of the minimum free-space oven is
favoured by most commercial laboratories.
American practice differs in that it involves drying the
coal at 104-110 C in an atmosphere of air, dried by passage
through sulphuric acid. Although the oven is required to
have a minimum amount of air space, this method is
probably only suitable for high-rank coals due to the risk of
oxidation in the drying process.
2.3.3
Volatile matter

The material referred to as volatile matter in a coal sample
represents the components of the coal, except for the
moisture content, that are liberated at high temperature in the
absence of air. This material may be released from the
organic compounds or from the mineral impurities, and the
significance of the latter should not be overlooked. If the
percentage of volatile matter is to be used to classify the
coal, correction for that derived from inorganic sources
(carbonates, clays etc.) must be made.
The volatile matter content is determined by heating the
coal under rigidly specified conditions. The percentage loss
of mass, less the percentage air-dried moisture, gives the
proportion of volatile matter present. British and Australian
Standards require the coal to be heated in a cylindrical silica
crucible in a muffle furnace of specified dimensions at
9005C for 7 min. American (A.S.T.M.) procedures,
involve heating at 95025C using a platinum crucible in a
vertical electric furnace. These differences in procedure give
slightly different results for the same coal, and the method
used must therefore be stated with the analytical results. A
modification of the A.S.T.M. procedure, involving a twostage heating process, is necessary for some low rank or
sparking coals.
2.3.4 Ash
The ash of a coal is the non-combustible inorganic residue
that remains when coal is burned. It represents the bulk of
the mineral matter in the coal, after volatile components
such as C02 (from carbonates), S02 (from sulphides) and H20
(from clays) have been driven off. As such, the ash makes up
a lesser proportion of the coal than does the total mineral
matter content.
Coals with a high ash content are generally less suitable
for utilization than low-ash coals. A greater mass of high-ash
material must be used to provide a given amount of heat or
other product due to the diluting effect of the noncarbonaceous components. Greater amounts of waste also
need to be removed after utilization.
Determination of ash content requires heating the coal in
a ventilated furnace, and expressing the mass of the residue
remaining as a percentage of the original coal. The heating
rate is normally slow at first, to prevent fixation of sulphur
or other compounds in the ash. In British and Australian
practice, the sample is heated slowly from ambient
temperatures to 815 C, where it is held until constant mass
is attained. A two-stage heating cycle, raising the
temperature first to 500 C, holding at that level for a
specified period and then heating at 815 C in a second
furnace may also be used.
American procedures depend on the nature of the
minerals present. In normal circumstances, the coal is heated
slowly to between 700 and 750 C and held at that
temperature until constant mass is developed. For coals that
have a high proportion of calcite and pyrite, a two-stage
process is required to prevent fixation of sulphur in the ash.

The coal is heated to 500 C over 1 h and 750 C over 2 h,
and held at 750 C until its mass becomes constant.
2.3.5
Fixed carbon
The fixed carbon content of a coal is the carbon found in the

material that remains after the volatile matter has been
expelled. It represents the decomposition residue of the
coals organic components, and carries with it small amounts
of nitrogen, sulphur, hydrogen and possibly oxygen as
absorbed or chemically combined material (Rees 1966).
The fixed carbon content is used as an index of the yield
of coke expected from a coal on carbonization, or as a
measure of the solid combustible material that remains in
coal-burning equipment after the volatile fraction has been
liberated. If corrections are applied for ash or mineral matter,
it may be used as an index of coal rank and a parameter in
coal classification.
Fixed carbon is not determined directly, but is simply the
difference, in an air-dried coal, between the sum of the other
components (moisture, volatile matter, ash) and 100%.
Appropriate corrections are made if the analysis is to be
reported to some other basis (Section 2.10.1).
2.4 ULTIMATE ANALYSIS

The organic component of a coal consists essentially of
chemical compounds made up from carbon, hydrogen,
nitrogen, oxygen and sulphur, and ultimate analysis involves
the determination of the percentage of each of these in the
sample. With the exception of nitrogen, these elements are
also found in many of the mineral species which occur in
coals, such as carbonates, sulphides, sulphates and hydrous
clay minerals. Hydrogen and oxygen also make up the total
or inherent moisture present in the coal being analysed.
Chapter 2
Carbon, hydrogen and oxygen are of great commercial

significance in assessing the coking, gasification and
liquefaction properties of the coal, while nitrogen and
sulphur represent possible sources of pollution in a coal to
be used for these or for combustion applications. The
percentages of carbon, hydrogen and oxygen in the organic
fraction of thecoal can also be used as indices of rank and as
parameters in coal classification.
2.4.1
Carbon and hydrogen
Carbon and hydrogen occur mainly as complex hydrocarbon

compounds. They are liberated as C02 and H20 when the coal
is burned, and as a result are most readily determined
together. However, the combustion process also liberates C0 2
from any carbonate minerals that may be present, and
additional H20 is derived from water in clays or other
hydrous minerals. Hydrogen is also found in the inherent
moisture of the air-dried coal, and thus any measure of the
total carbon and hydrogen includes a certain amount of
material derived from inorganic sources. Corrections and
separate analyses can be made to allow for the inorganic
material.
Most techniques for the determination of carbon and
hydrogen are based on heating the air-dried coal in a stream
of dry oxygen, and collecting the C02 and H20 produced in a
series of absorption tubes. However, oxides of nitrogen and
sulphur, as well as possibly small amounts of chlorine are
also produced by the combustion process, and provision
must be made in the apparatus to ensure they do not interfere
with the selective absorption system.
Two methods of determination are covered by standard
procedures in Britain and Australia. These are the Liebig
method {Fig. 2.5), where the coal is heated to 800 C, and
the high temperature method, where it is heated to 1350 C.
The high temperature method requires fewer additional
processes to allow for sulphur, nitrogen etc. and is favoured
by many commercial laboratories. American (A.S.T.M.)
standards provide only for the Liebig method to be used.
2.4.2
Nitrogen
The nitrogen found in coals appears to be mainly confined to

the organic compounds present. The nature of these
compounds, and their origin, isdiscussed by Francis (1961).
No nitrogen-bearing minerals are known in coals, but some
nitrogen compounds may occur in pore waters, especially in
brown coals.
In the carbonization process used to manufacture coke,
some of the nitrogen reacts to form ammonium compounds.
These may be extracted as a by-product for use as fertilizer,
or in the manufacture of nitric acid. Similar ammoniacal
compounds are also formed in liquefaction or gasification
operations, using hydrogen that would otherwise form the
more valuable hydrocarbon products. On combustion of the
coal, the nitrogen helps to form oxides which may become
atmospheric pollutants when the flue gases are released, and
as a result the use of coals with a low nitrogen content is
often preferred.
The most commonly-used technique for nitrogen
determination is the Kjeldahl method, which converts the
nitrogen in the coal to ammonium sulphate by catalytic
digestion in sulphuric acid. The amount of ammonium
sulphate formed is then determined by a series of titration
processes.
2.4.3 Sulphur
Sulphur may occur in coal in a number of ways:
(a) Organic sulphur, where it is incorporated into the
hydrocarbon compounds of the coal substance.
(b) As sulphide minerals, such as pyrite, in the inorganic
fraction (pyritic sulphur).
(c) As sulphate minerals, mostly hydrous iron or
calcium sulphates, usually produced by atmospheric
oxidation of these sulphides.
In ultimate analysis, the total sulphur content is
determined, representing material occurring in all these
possible forms. For many purposes, however, the relative
amount of sulphur in each form is also needed, and this can
be determined by a separate analytical procedure (Section
2.5.1). Even if the complete ultimate analysis is not
performed, total sulphur determination is nearly always
carried out, along with proximate analysis, on a coal being
evaluated for commercial purposes.
Copper
Dry Cpal
oxygen
gauze
sample
Copper
oxide
Lead
chromate
l...........1-1
1 (80CCC)
Furnac
e no.
Start
2 (800C)
Silver
gauze
C02 and H20
I to
:
3 (600C)
absorption
tubes
Finish
Fig. 2.5 Schematic diagram showing combustion tube for determination of carbon and hydrogen by the Liebig method. The copper oxide
ensures complete conversion of carbon monoxide to carbon dioxide, the yield of which is measured in the absorption tubes. Oxides
of sulphur are retained by the lead chromate, and chlorine by the silver gauze, preventing interference with the absorption process.
The tube is 1.22 m long. (After BS 1016, part 6, 1977.)

Coals with a high sulphur content present numerous
problems on utilization. In combustion applications, the
sulphur gives rise to corrosion problems in the boiler, and to
build-up of insulating deposits (fouling) on the boiler tubes.
It also causes problems with atmospheric pollution as large
amounts of S02 are released with the stack gases. Installation
of limestone-based stack gas scrubbers may be necessary for
the plant to conform to environmental regulations.
Part of the sulphur is carried through to the products of
liquefaction, gasification and coking operations. It must be
removed at some stage of the liquefaction or gasification
process, or similar atmospheric pollution and corrosion
problems will arise when these products are used. An
unacceptably high level of sulphur may also be passed on to
the iron and steel produced using coke from high-sulphur
coals, resulting in material which is brittle or difficult to
weld. The sulphur may be removed in the blast furnace (at
additional cost) by producing additional volumes of slag, or
by oxidation in the subsequent steel-making process.
The total sulphur content of a coal may be determined by
one of several methods that convert it to sulphate for wet
chemical analysis. One of these, the Eschka method,
involves oxidation of the coal at 800 C in magnesium oxide
and sodium carbonate, followed by addition of barium
chloride to form insoluble barium sulphate. The mass of
barium sulphate formed gives the total sulphur content of the
coal. Another is the high temperature method where the
coal is burned in oxygen at 1350 C, converting all the
sulphur present to S02. The S02 is then converted to sulphuric
acid for titrimetric determination (Fig. 2.6).
Other methods that may also be used, although giving a
lesser degree of precision in the determination are:
(a) Analysis of washings from the bomb calorimeter, used
in specific energy determinations (Section 2.7.1).
(b) X-ray fluorescence or similar analysis, under

appropriate conditions of the whole coal sample.
The analysis of washings from the bomb calorimeter is
included as an alternative to the Eschka and high
temperature methods in American (A.S.T.M.) standard
procedures.
2.4.4
Oxygen
Oxygen is a component of many of the organic compounds

in a coal. It is also found in the moisture, and in many of the
mineral species, such as clays and carbonates. If the coal is
not fresh, it may be found in iron oxides, hydroxides and
various sulphate minerals, as well as oxidized organic
compounds.
When corrected for the component found in moisture and
mineral matter, the oxygen in a coal is important as an
indicator of rank. It is one of the main parameters used in
some coal classifications (Section 2.10.2). Oxygen is also of
great significance in gasification and liquefaction operations,
as it takes up much of the hydrogen otherwise used to
produce hydrocarbon compounds.
The oxygen content of a coal is traditionally determined
by subtracting the amount of other chemical components (C,
H, N and S) from 100%. Techniques involving direct
determination are also available, which avoid the effect of
cumulative error in the analysis by difference. These
methods involve heating the coal in an inert atmosphere at
temperatures of at least 900 C (Rees 1966) or up to nearly
2000 C (Kinson & Belcher 1975), liberating the oxygen as
carbon monoxide. The monoxide is then converted
catalytically to C02, the amount of which is determined in an
absorption train to give the coals oxygen content.
2.5 MISCELLANEOUS CHEMICAL ANALYSES

As well as proximate and ultimate analysis, a range of other
chemical tests is often carried out on coal
Furnace (1350C)
Fig. 2.6 Determination of total sulphur by the high temperature method. (After Br.tish Standard
1016, Part 6, 1977.)
10
Chapter 2
samples. Some of these tests are used to enable correction of

proximate and ultimate analysis data to allow for the mineral
matter constituents, while others are used to evaluate the
coals suitability for specific purposes. A comprehensive
summary of analytical procedures that may be used for
industrial or research applications is given by Karr (1978).
2.5.1
Forms of sulphur
Although the total sulphur content provides sufficient data

for most commercial applications, a knowledge of the
relative amounts present in each of the three principal forms
is useful for the following purposes:
(a) To assess the level to which the total sulphur content
might be reduced by coal preparation processes. It is
possible that a preparation plant will remove much of the
pyritic and sulphate sulphur, but such a plant is unlikely to
reduce the organic sulphur content.
(b) To assess, by normative calculation, the amount of
mineral matter in the coal. This is based on formulae using
the ash content of the coal and several other chemical
properties (Section 2.9.2).
Determination of the amount of sulphate sulphur in the
coal is based on solution of the sulphates in hydrochloric
acid, and their precipitation as barium sulphate for
gravimetric determination. The total iron content of the
sulphate fraction is also determined for use in the analysis of
pyritic sulphur.
The amount of pyritic sulphur in the coal is determined
by dissolving both sulphates and sulphides in nitric acid, and
determining the total iron content of the solution. The
amount of iron (and hence sulphur) in the sulphide fraction
is then determined by subtraction of the amount of iron
liberated in the analysis of the sulphate sulphur content.
The organic sulphur content of the coal is determined by
subtraction of the sulphur present in these two forms from
the total sulphur content determined in ultimate analysis.
2.5.2
Carbonate carbon dioxide
Carbonate minerals, principally calcite, dolomite, ankerite

and siderite, are a common constituent of many coals. These
minerals liberate C02 on combustion, and therefore
contribute to the total carbon content of the coal as
determined by ultimate analysis. However, this process is an
endothermic reaction, and reduces the amount of energy
available from a coal otherwise apparently having a high
carbon content. Knowledge of the amount of this carbon is
necessary for the following purposes:
(a) Determination of the amount of combustible carbon
from the total carbon content. This is required to give a
detailed assessment of the coal in all areas of potential
usage.
(b) Estimation of the percentage of mineral matter by
calculation (Section 2.9.2). Knowledge of the carbonate C02
content assists in calculation of the mineral matter content

from the amount of ash residue by normative methods, and
also enables adjustment of the volatile matter content to
assess that fraction derived solely from the coals organic
component (Section 2.10.1).
The carbonate C02 content is determined by solution of
the coal in hydrochloric acid and measuring the amount of
C02 produced. This may be done either by a gravimetric
method using an absorption train, or a titrimetric method
using benzylamine and potassium methoxide. A manometric
method based on measuring the pressure increase in a closed
vessel may also be used for high rank (hard) coals.
2.5.3
Chlorine
Small amounts of chlorine are commonly present in coals,

either as inorganic salts (e.g. NaCl, KC1) in the mineral
fraction, or as a component of the organic matter. In
combustion applications, this chlorine may cause corrosion
and fouling of boiler equipment and also possibly contribute
to atmospheric pollution. Knowledge of the chlorine content
is necessary to apply corrections in other analyses, such as
specific energy and total sulphur determinations. It is
included in the amount of oxygen in ultimate analysis as
determined by difference, and must be allowed for in
assessing the percentage of mineral matter from the ash
content in some normative calculations.
Chlorine may be determined by the Eschka method,
where the coal is oxidized at 675 C in magnesium oxide
and sodium carbonate. The chlorine is converted to chlorides
which are then analysed by titration.
As an alternative, American procedures allow for the
combustion of the coal, together with the MgO and Na 2C03,
in a bomb calorimeter. The chlorine is determined by
analysis of the bomb washing solutions.
More commonly, chlorine is analysed in conjunction with
the determination of total sulphur by the high temperature
method. The coal is burned in oxygen at 1350 C, and the
liberated chlorine absorbed in hydrogen peroxide to form
hydrochloric acid. This can then be analysed titrimetrically
at the same time as the sulphur (sulphuric acid) formed by
the combustion process.
2.5.4. Phosphorus
Small amounts of phosphorus are also found in some coal
samples. Most of this appears to be concentrated in the
mineral matter, either as apatite (Ca5 (P04)3 (F, OH), or a
member of the goyazite group (SrAl3 (P04)2(0H)5). Large
quantities of phosphorus are undesirable in coking coals, as
it is carried over and contaminates the final steel product.
Chemical analysis for phosphorus is based on oxidation
of the coal in strong acids, or on acid solution of the coal ash
followed by spec- trophotometric determination with
ammonium molybdate. Phosporus contained in the acidinsoluble goyazite minerals could be overlooked,
particularly by the first technique, and methods such as
emission spectroscopy or X-ray fluorescence may be
necessary in some cases as alternatives.
2.5.5
11
Coal ash consists almost entirely of the decomposed residues

of silicates, carbonates, sulphides and other minerals, and at
least 99% of its chemical composition can usually be
expressed in terms of the same metal oxides as that of other
crustal rocks. The composition of the ash gives a useful
guide to the types of minerals present in the coal. Such data
are also of commerical significance in coking coals, as the
ash of coke plays a part in the formation of blast furnace
slag, and infuel coals to indicate boiler fouling or ash
viscosity characteristics.
The ash may be dissolved by various means, treated with
appropriate reagents and the resulting solutions analysed
using either an optical absorption spectrophotometer or a
flame photometer (Fig. 2.7). Alternatively, techniques such
as atomic absorption spectrophotometry, emission
spectroscopy or X-ray fluorescence may be used for the
analysis process.
Ash analysis
2.5.6
Trace elements
Apart from the major organic and inorganic constituents,

coals contain a variable assemblage of elements in trace
amounts. Some of these are more abundant in the less dense
fractions of the coal, separated by float-sink methods
(Section 2.6.3), and appear to be incorporated mainly with
the organic components. Others are concentrated in the
dense, mineral-rich material, and appear to have a dominant
inorganic affinity (Gluskoter et a! 1977; Ward 1980). They
may represent either metallo-organic compounds in the coal
structure, minor amounts of a mineral with an abundance of
the particular element (e.g. zinc in sphalerite) or major
amounts of a mineral in which the element itself occurs in
trace proportions (e.g. manganese in ankerite).
12
Chapter 2
In some areas, the trace elements may be useful as aids to

seam correlation or as indicators of the coals depositional
environment. Boron, in particular, appears
S02
Aro, Na20 K,0
Fe20,
TiO,
Mn,0
P,0,
CaO
MgO
SO,
Fig. 2.7 Flowsheet illustrating the analysis of coal ash using optical absorption spectrophotometer, flame photometer, titration and gravimetric
techniques. (After British Standard 1016, Part 14, 1963.)
13

to be more abundant in coals influenced by marine
conditions (Swaine 1962; Bohor & Gluskoter 1973).
A number of the trace elements may be transferred to
hydrocarbon liquids, coke and other products when the coal
is used. They may act as catalysts or inhibitors in some of
the complex processess of coal conversion.
Trace elements may also be released to the environment,
either by combustion of the coal or its products or by
weathering of coal ash and colliery waste material. The
elements involved include many that are essential to
biosphere processess, as well as those that are toxic, in
certain forms, to plants, animals and man. High
concentrations of critical elements, such as lead, arsenic,
cadmium and mercury, may limit the suitability of a coal for
use in sensitive situations. In other cases, the trace elements
may represent potentially valuable by-products from the
materials
concerned.
Most trace element determinations are made by optical
emission or atomic absorption spectrometry of the coals
ash, supported in some cases by techniques such as X-ray
fluorescence and neutron activation analysis (Gluskoter et al
1977). The ash may be prepared by radio-frequency
oxidation, a technique that destroys the organic matter at
temperatures below 150C (Section 2.9.2), or by heating the
coal in air under various conditions, including the processes
normally used in proximate analysis. Special precautions are
sometimes taken to limit the loss of volatile inorganic
elements (Ruch et al 1974). The results are expressed either
as a proportion of the ash itself, or as a proportion of the
original air-dried coal. An indication of the trace elements in
a range of Australian and North American coals is given in
Table 2.1.
TABLE 2.1 Trace elements in Australian (Swaine 1977)* and American (Gluskoter et al 1977) coals
Australia
Concentration (p.p.m. air-dried coal) U.S.A.
Illinois Basin Range Mean*
Appalachians Range Mean*

Element
0.02-0.08
1.0-120
12-230
5.0-750
0.5-4
0.1-65
2.0-34
0.03
14
110
100
1.7
2.2*
7.3
0.01-0.06
1.8-100
5.0-120
72-420
0.23-2.6
0.10-0.60
1.5-33
4.0-60
5.0-44
29-140
0.8-10
1.0-43
0.03-1.6
18
14
67
3.2
10-90
5.1-30
50-150
2.9-11
6.9
0.2
6.8
53
0.10-6.0
0.05-0.47
8.1
21
64
32
2.7
2.2
3.8
0.10-22
6.3-28
15-1500
1.0-18
1.6-9.3
1.1-8.1
0.20-8.0
28-550
1.8-9.0
2.7-20
6.0-210
0.3-29
7.6-68
10-340
0.8-220
1.2-7.7
0.4-7.7
0.2-51
10-130
0.71-5.1
0.31-4.6
11-90
0.04-4.2
10-5300
12-130
35
2.1
1.5
32
0.82
250
47
6.1-23
2.4-61
0.40-2.9
14-73
0.22-1.2
2.0-120
8.0-88
0.02
Ag
25As
42B
200
Ba
1.3Be
0.24*
Cd
9.8Co
20Cr
18Cu
89F.
5.7Ga
1.6Ge
0.20
Hg
15La
18Mn
4.6Mo
15Ni
150
P
5.9Pb
5.1Sc
4.0Se
2.0Sn
130
Sr
4.5Th
1.5U
38V
0.69
W
25Zn
45Zr
Western coals Range Mean*
N.S.W. and Qld Range Mean*
0.01-0.07
0.34-9.8
0.03
2.3
<0.2-1
<1-55
<0.5
3
16-140
160-1600
56
500
1.5-300
<40-1000
60
<100
0.10-1.4
0.10-0.60
0.6-7,0
<0.4-8
0.05-0.2
< 0.6-30
1.5
0.10
4
2.4-20
3.1-23
19-140
0.8-6.5
0.46
0.18*
1.8
9.0
10
62
2.5
< 1.5-30
2.5-40
15-500
1-20
6
15
80
4
0.10-3.0
0.02-6.3
0.91
0.09
<0.3-30
0.026-0.40
1.8-13
1.4-220
0.10-30
5.2
49
<4-50
2.5-900
<0.3-6
6
0.10
10
150
1.5
0.8-70
30-4000
1.5-60
<0.3-30
0.21-2.5
<0.9-15
15
310
10
3
0.79
<3
1.5-18
10-510
0.7-9.0
0.50-4.5
0.40-2.7
0.10-15
2.1
5.0
130
3.4
1.8
1.4
1.9
93-500
0.62-5.7
260
2.3
< 201000
<0.2-8
100
2.7
0.30-2.5
4.8-43
0.13-3.3
1.2
14
0.75
0.4-5
4-90
< 4-20
2
20
<10
0.30-17
12-170
7.0
33
12-73
6-400
25
100
* Updated 1980.
* Arithmetic mean.
* Numerous values below detection limit.
14
2.6
Chapter 2
MISCELLANEOUS MECHANICAL TESTS
Apart from chemical analysis, the commercial evaluation of

a coal also involves the determination of a number of its
physical properties. These include the relative density, and,
for samples of broken coal, the particle size distribution. In
addition, because much of the coal produced from modern
mines is treated in a preparation plant prior to sale, a brief
summary is given in this chapter of float-and-sink
washability tests. Although the technology of coal
preparation is more fully discussed in Chapter 8, float-sink
testing is included at this point because much of the more
comprehensive analysis is normally carried out on fractions
separated out by such methods to simulate washed coal
products.
2.6.1
Relative density
The relative density (or, less correctly, the specific gravity)

of a coal depends on the rank of the material and the degree
of mineral impurity. Knowledge of the relative density of
each ply is necessary for the preparation of composite
samples representing larger intervals of the seam. It is also
an essential factor in conversion of coal reserves from units
of volume to units of mass.
Determination of relative density is normally based on
the loss of weight when the sample is immersed in water. For
large particles, including samples of drill core prior to
crushing, a certain amount of air remains in the pores of the
coal, and the value determined is called the apparent
relative density. The true relative density is best determined
from the volume of a known mass of fine coal (e.g. crushed
to less than 210 /m) by means of a standard relative density
bottle or pycnometer.
For coals of equivalent rank and similar type, the relative
density, or even the apparent relative density, is essentially
proportional to the ash content (Fig. 2.8). Once the actual
relationship has been established for the coals of a given
exploration area, a general assessment of the broad nature of
the seam can be made before detailed testing is carried out.
The selection of intervals for detailed analysis can be
aided by a profile of the apparent relative density throughout
the seam. In areas remote from laboratory facilities, much
useful information can also be obtained from the
determination of apparent relative density in the field
(Alpern 1977). This gives exploration staff immediate access
to at least some coal quality data, and enables aspects of
exploration programmes to be recast if necessary without
waiting for laboratory results.
2.868
Fig. 2.8 Relationship of relative density to ash content for

coals and carbonaceous shales in the Agades Basin. (Alpern
1977.)
2.6.2
Particle size distribution
The distribution of particle sizes in a broken coal depends

on the mining, crushing and handling processes it has
undergone, together with the hardness, tenacity and degree
of fracturing in the material itself. Because the different
items of coal preparation equipment work best only with
certain sized coal particles, the size distribution of the coal
is a critical factor in plant design. Similarly, many types of
equipment that use coal also require the material to be
supplied with particular size distribution characteristics.
Determination of particle size distribution is based on
methods of sieve analysis similar to those for other
geological and engineering materials. The results are
normally tabulated as shown in Table 2.2, and a graphic
representation using appropriate axes may be included as
well (Section 8.2.3). The graphic plot enables computation
of the various size-distribution parameters, such as the
mean particle size and a measure of the degree of size
variability.
It is usually essential that an estimate of the size
distribution of mined coal be made in an area under
commercial development well before mining actually takes
place. This information is needed to enable effective
design of the accompanying coal preparation plant. Such
information is normally gained by a trial mining operation,
or if this is not possible, by a series of crushing and
tumbling tests on large diameter bore cores (Proudfoot
1977). Prediction of size distribution in this way is
discussed more fully in Section 8.2.3.
2.6.3
Float-sink testing
As well as being of different sizes, the particles in a mass

of broken coal are all of different relative
15

TABLE 2.2 Sieve analysis data for a crushed coal.
Mass retained
Cumulative
Cumulative
Particle
Size fraction
(mm)
in size
fraction (%)
percentage
oversize
percentage
undersize
size
(mm)
- 125 + 63.0
4.8
- 63.0 + 31.5
- 31.5 + 16.0
- 16.0 + 8.00
12.2 .
20.6
18.2
9.2
0
4.8
17.0
37.6
100
95.2
83.0
62.4
55.8
65.0
72.2
79.4
44.2
35.0
27.8
20.6
- 8.00 + 5.60
- 5.60 + 5.00
- 4.00 + 2.80
- 2.80 + 2.00
7.2
7.2
4.3
- 2.00 + 1.00
- 1.00 + 0.50
6.7
4.6
- 0.50
5.0
: 83.7
density. The denser particles, of course, represent material

with a high ash or pyritic sulphur content. The purpose of
commercial coal preparation is to remove these, so that the
overall ash or sulphur content of the mined product is
reduced to an acceptable level.
Except for froth flotation, oil agglomeration and similar
processes used on fine-grained particles, most coal
preparation equipment segregates the materials supplied on
the basis of their relative density. Floatsink testing in the
laboratory determines the density distribution of particles in
the sample by immersion of the broken coal in liquids of
known relative density. Further studies, such as ash, specific
energy or swelling number determinations, may also be
carried out on the coals floating and sinking in each liquid
used.
The liquids used in float-sink testing generally have
relative densities ranging from 1.30 to 2.00. Mixtures of
organic liquids such as tetrabromoethane (R.D. 2.89)
perchlorethylene (R.D. 1.60) and toluene (R.D. 0.86) are
normally preferred because of their low viscosity and rapid
drying characteristics. In some cases, however, these may
interfere with the results of coking tests subsequently
performed on the coal, and inorganic liquids, made up of
aqueous solutions with varying concentrations of salts such
as zinc chloride, may be used instead.
The coal is immersed firstly in the liquid with the lowest
R.D., with the floating fraction being skimmed off, weighed
and analysed. The sinking fraction from this test is
transferred to the next liquid in the series and the operation
repeated.
90.4
95.0
16.3
9.6
5.0
125
63.0
31.5
16.0
8.00
5.60
4.00
2.80
2.00
1.00
0.50
The results may be plotted graphically as a series

ofwashability curves (Section 8.2.4), These represent the
percentage of material floating or sinkingcalculated on a
cumulative basis, plotted against the ash content of that
material, and also show the percentage of the sample floating
plotted against the relative density of the liquid in which it
was tested. From these and other data, it is possible to
estimate the yields of coal and refuse that would be produced
to give a floating fraction with a specified ash content, as
well as the relative density required to achieve such a
separation.
Float-sink testing is normally carried out on samples of
mine products or preparation plant feedstocks. Other types of
samples, particularly those obtained from bore cores, are
generally subjected to some form of comminution prior to
testing, to provide a mass of broken coal that simulates these
materials. This may range from simple crushing for slim (50
mm) cores to a series of controlled breaking and tumbling
operations on large diameter (150-200 mm) cores to simulate
the mining and handling process. Fine coal (e.g. that passing
a 0.5 mm sieve) is often separated out from the broken mass
prior to testing, as this is normally dealt with in the
preparation plant by processes, such as froth floatation, that
do not depend on density contrasts.
A reconstituted preparation plant product may be
obtained by combining relevant proportions of the required
floating fractions from the coarse coal and the clean
material derived from any fine coal component. Testing of
this material, and not the original whole coal sample,
allows the results to describe more closely the marketed
product, rather than the raw coal going from the mine to the
preparation plant. Laboratory float-sink testing, however,
does not necessarily duplicate the action of full-scale coal
preparation equipment and care must be taken in the use of
data gained in this way.
16
Chapter 2
2.6.4
Shale breakdown test
'
Many of the rock types that form the roof, floor or intraseam bands of coal seams tend to disintegrate when exposed
to water. This gives rise to problems with coal extraction
(e.g. weakening of roof or overburden strata), and also with
aspects of coal washery operation. Fine clay, for example,
may become suspended in the water used to clean the coal,
altering its density and hence the effectiveness of float-sink
separation. It may also form a film on the clean coal
particles, raising the ash content of the plant product to some
extent.
Such behaviour is commonly due to an abundance of
expandible lattice clay minerals such as montmorillonite in
the non-coal components. An indication of the degree to
which individual beds or seam composites may cause
difficulties can be gained by a standardized procedure (e.g.
Australian Standard 1661), where a sized sample is tumbled
in water for a specified period. The amount of shale
breakdown is obtained from the proportion of fine material,
determined by sedimentation analysis of the residue at the
conclusion of the tumbling process.
2.7
SPECIAL TESTS FOR COMBUSTION
Apart from chemical analysis, including assessment of the

level of potential atmospheric pollutants in the coal, a
number of other tests are carried out on coals to be used for
steam-raising or other processes involving combustion.
Foremost among these is determination of the specific
energy or calorific value of the coal, a measure of the
amount of heat energy available per unit mass. Other tests of
significance include the investigation of the properties of the
coals ash at high tempertures, and the ease with which it is
possible to reduce the coal to fine powder for pulverized-fuel
applications. Further analyses, such as assessing the degree
of abrasion on the equipment grinding the coal, may be
carried out in some circumstances as well.
2.7.1
Specific energy
The energy liberated by a coal on combustion is chiefly due

to the exothermic interaction of its hydrocarbon compounds
with oxygen. Other materials in the coal, such as nitrogen,
sulphur and the mineral matter also undergo chemical
changes in the combustion process, but many of these
reactions are endothermic and act to reduce the total amount
of energy otherwise available.
In an operating furnace, the combustion is unconfined.
Water vapours and other compounds (acid forming gases)
escape directly to the atmosphere without condensation. In
the laboratory, however, combustion takes place under
confined conditions, and most of the products are allowed
to condense after ignition. This causes the total amount of
energy given off by the coal to be increased due to the
latent heat given off in the process, and the result, known

as the gross specific energy, usually represents an overestimation of the amount of heat actually liberated from
the coal under operating conditions.
The heat given off per unit mass of coal in unconfmed
conditions is called the net specific energy. It differs most
significantly from the gross value in coals, such as brown
coals or lignites, that have a high moisture content. The net
specific energy can be evaluated by correction of the
laboratory- determined gross value, based on factors such
as the moisture, sulphur and chlorine contents of the coal
concerned.
Laboratory-determined values of net or gross specific
energy are usually also based on air-dried coal, and may
even be quoted after recalculation to a dry or dry ash-free
basis. The amount of total moisture in the coal as supplied
to the furnace must be taken into account as well, giving a
net wet specific energy which represents the actual heat
output from the coal in commercial utilization.
Specific energy is determined by ignition of the coal
under controlled conditions in a calorimeter. The most
widely used type of apparatus is the adiabatic bomb
17
calorimeter, illustrated in Fig. 2.9, but an isothermal bomb

calorimeter may also be employed. A small amount of coal
is ignited electrically, in an oxygen atmosphere, within a
pressure-resistant metal cylinder or bomb (Fig. 2.10).
This cylinder is immersed, before firing, in a known mass
of water, and the increase in temperature of this water is
monitored after combustion takes place. The amount of
heat given off by the sample is determined from the
temperature rise by reference to previous calibration runs
with a thermochemical standard such as benzoic acid in
place of the coal.
In order to prevent heat losses in the adiabatic .
instrument, the calorimeter containing the bomb is
surrounded by a second water jacket, kept at the same
temperature as the water in the calorimeter itself by
thermistor-controlled heating elements. Small corrections are
made to the temperature rise based on the calibration curve
of the thermometer, and to allow for the heat generated by
the firing wire. Other corrections are applied, based on either
the sulphur and nitrogen contents of the coal, or on the
results of chemical analysis of the bomb washings, to allow
Ash fusion temperatures are determined by viewing a

Chapter 2
moulded specimen of finely ground ash through an
Rubber
ring
Fig. 2.10 Cross-section of calorimeter bomb.
observation window in a high-temperature furnace. The

moulded ash, usually in the form of a cube or a pyramid, is
heated steadily from 1000 C to as high a temperature as
possible, preferably around 1600C. The following
temperatures are recorded (Fig. 2.11).
Fig, 2,9 Adiabatic bomb calorimeter.
for the heat of formation of nitric and sulphuric acids in

the laboratory operation.
The results of specific energy determinations are
expressed in the SI system of units as megajoules per
kilogram (MJ kg-1). Other units also used for specific
energy or calorific value are calories per gram,
kilocalories per kilogram and British thermal units per
pound. Conversion factors for these units are:
1.00 MJ kg'1 = 429.923 BTU lb"1
= 238.846 cal g_1 or kcal kg-1
2.7.2
Ash fusion temperatures
The behaviour of the coals ash residue at high

temperatures can be a critical factor in selection of coals
for combustion applications. Most furnaces are designed
to handle and remove the ash as a powdery solid, and a
coal with an ash that fuses into a viscous liquid and sets to
form a hard clinker on cooling is unsatisfactory in this
type of equipment. Special furnaces can be designed,
however, that actually require the ash to fuse, allowing it
to be removed from the apparatus as a clinker or even in
liquid form. In such cases a coal with a high ash fusion
temperature would be inappropriate.
(a) Deformation temperature

This is reached when the corners of the mould first become
rounded.
(b) Softening (or sphere) temperature
This is reached when the top of the mould takes on a
spherical shape.
(c) Hemisphere temperature
This is reached when the entire mould takes on a
hemispherical shape.
Chapter 2
2
3
4
5
Fig. 2.11 Profiles of pyramid specimens at critical points in ash fusion determination. (1) Original specimen.
(2) Deformation temperature. (3) Sphere temperature. (4) Hemisphere temperature. (5) Flow temperature.
1
20
Chapter 2
(d) Flow (or fluid) temperature

This is reached when the fused ash collapses to a flattened
button on the furnace floor.
All of these temperatures are usually quoted together,
indicating the range over which the fusion of the ash takes
place. Furher information can be gained on ash fusion
properties by varying the atmosphere in which the
specimens are heated. A reducing, semi-reducing or
oxidizing atmosphere may be made up from appropriate
gases, to duplicate the plant operating conditions. In
addition, since the ash sample is placed on a ceramic tile for
the test, any interaction between the fused ash and
comparable furnace linings may also be investigated.
The behaviour of the ash at high temperature is related to
its chemical composition (Huffman et al 1981). Material
with a high proportion of aluminium generally appears to be
the most refractory. Small amounts of iron, calcium and
potassium, however, if present, may act as fluxing agents
and reduce the temperature at which fusion occurs.
2.7.3
Hardgrove grindability index
Most modern coal-burning equipment requires the coal to be

ground to a fine powder (pulverized) before it is fed into the
combustion chamber. The ease with which this can be
accomplished depends on the strength or tenacity of the
coal, and is measured by the Hardgrove grindability index.
In this test, a given mass of coal with a fixed particle size
distribution is ground in a specified way in a standardized
ring-ball mill (Hardgrove mill). The resulting powdered coal
is screened and the Hardgrove grindability index (H.G.I.)
calculated from the mass of fine material produced.
Coals with a high Hardgrove index are relatively soft
and easy to grind. Those with a low value (less than 50), are
hard and much more difficult to make into pulverized fuel.
A greater number of grinding mills is needed in plants that
use such coal if a given through-put of material is to be
maintained.
2.7.4
Abrasion index
Coarse particles of hard mineral matter, such as quartz, can

cause significant abrasion of grinding surfaces in the
pulverizing equipment associated with many coal-burning
furnaces. The likely extent of this abrasion can be tested by
allowing a sample of coal, with a specified size distribution,
to be agitated for 12 000 revolutions at 1 500 rev. min 1 in a
special mill equipped with four metal blades (Yancey et al
1951). The abrasion index is determined from the loss in
mass of these blades, and is expressed in milligrams of
metal per kilogram of coal involved.
2.8 MISCELLANEOUS TESTS FOR

CARBONIZATION
Cabonization is the process of heating coal at a temperature

of several hundred degrees centigrade in the absence of air
to produce the following types of material:
(a) A carbon-enriched solid, called coke if vesicular
and fused or char if less porous or not fused;
(b) Liquid products, made up of a mixture of
hydrocarbons called tar and aqueous solutions containing a
variety of dissoved materials called ammoniacal liquor;
(c) Hydrocarbon and other compounds that remain in the
form of gas on cooling to normal temperatures.
Carbonization is the basis for the manufacture of coke,
and also of many liquefaction and gasification techniques.
The relative amount of each type of product that can be
derived from a given coal depends on its petrographic
features (Chapter 4), and on details of the carbonization
process employed. An evaluation of the yield of each of
these materials on carbonization can be made by tests such
as the Gray-King assay and the Fischer assay, which also
produce samples of the products for further testing.
The most significant use of carbonization processes is in
the manufacture of coke for metallurgical operations. A
number of tests may be used to evaluate the suitability of a
coal for coke production (Zimmerman 1979), and many of
these are carried out in the early stages of quality
assessment. If the results of these tests are encouraging,
more sophisticated investigations such as pilot plant coke
oven tests can be applied to larger samples at a later stage.
2.8.1
Crucible swelling number (Free
swelling index)
The most simple test to evaluate whether a coal is . of
potential value for coke manufacture is to determine the
crucible swelling number or free swelling index. This test
involves heating a small sample of crushed coal in a
standardized crucible to a temperature of around 800 C. An
apparatus as shown in Fig. 2.12 is normally employed, but
electric heating methods are also available for the process as
an alternative.
After heating for a specified time, or until all of the
volatiles have been driven off, a small coke button remains
in the crucible. The cross-sectional
21
Fig. 2.12 Apparatus for the determination of Crucible

Swelling Number (Free Swelling Index). (From A.S.T.M. Standard D-720, 1967.)
exposed to weathering, or even coals that have been
Fig. 2.13 Characteristic profiles of coke buttons for different values of the Crucible Swelling Number (Free Swelling Index). (From British
Standard 1016, part 12, 1980.)
profile of this coke button, compared to a series of standard

profiles (Fig. 2.13), determines the swelling number of the
coal. The coke button of a coal that does not swell, however,
requires further simple testing for strength before the value
is finally determined.
A coal with a very low swelling number (0-2) is not
particularly satisfactory in itself for coke manufacture, as
the coke formed has too low a porosity, and hence too little
surface area on which any reaction can take place during
use. Where a single coal acts as the raw material, a high
swelling number (8-10), however, is also undesirable. The
coke made from such coals is usually too weak, due to the
thin walls of its pores, to support the loads imposed on it in
the blast furnace. In these circumstances the coal should
ideally have a swelling number of between 4 and 6, to give
the coke the right combination of porosity and strength.
Since most coke is manufactured from blends of several
coals, however, each with different swelling characteristics
(Section 4.3), coals with a value outside this range,
particularly those with a high swelling number, may still be
of considerable value.
The swelling number is significantly affected by the
particle size distribution of the sample, and also by factors
such as the heating rate. Like most other coking properties,
it may also be reduced by oxidation. Coals that have been
improperly stored, may show a marked deterioration in

swelling properties, and testing should be carried out as
soon as possible after the sample is prepared.
2.8.2
Gray-King carbonization assay and
coke type
The total amount of solid, liquid and gaseous products given
off from the coal by carbonization may be determined by the
Gray-King assay. In this test, the coal is heated in a sealed
cylindrical retort tube, laid horizontally, from 300 to 600 C
in 1 h for low temperature carbonization or from 300 to 900
C in 2 h for high temperature carbonization. The tars,
liquors and gases are collected and the yield of each product
is determined along with the mass of coke formed. Further
analysis of these materials may also be carried out if
required.
Low temperature (600 C) carbonization best measures
the products of primary decompostion, and specifically
characterizes the coal. High temperature carbonization
measures the products of secondary decomposition. It is
more useful in the practical sense, since it correlates better,
though still not exactly, with industrial carbonization
processes.
With coking coals, the low temperature Gray-King assay
may be modified to produce the coke without collection and
22
Chapter 2
analysis of the other carbonization products. This coke, in

the form of a semi-cylindrical rod, is then examined to
determine the Gray-King coke type (Table 2.3). The coal
may remain in powder form, either granular or weakly
coherent (coke types A, B, C) or it may be fused, but
reduced in volume (coke types D, E, F). Coal that retains its
original volume and forms a strong, well fused product is
classified as having coke type G. If it swells beyond that
volume, a series of additional tests is run using various
amounts of electrode carbon mixed with the coal. The coke
type is determined from the proportion of this material
needed to produce a coke with type G characteristics (coke
type Gi and above).
Although it is not determined under the same conditions,
the Gray-King coke type corresponds
23

TABLE 2.3 Characteristics for classification of Gray-King coke type. (From British Standard 1016, part 12, 1980.)
A, B and C
D, E and F
Retains initial cross section
Shrunken
Examine for strength
Non-coherent
Barely coherent
Coherent
Moderately hard
and shrunken
Hard and very

shrunken
Usually in powder
form but may contain some pieces
which, however,
cannot be handled
without breaking
In several pieces
and some loose
powder. Pieces
can be picked up
but break into
powder on
handling
Usually in one
piece but easily
broken; may be
in two or three
pieces with
practically no
loose powder;
very friable and
dull
May be fissured
Usually very
but can be
fissured; moderate
scratched with
metallic ring when
fingernail and
tapped on a hard
stains the fingers
wooden surface;
on rubbing the
does not stain the
curved surface
fingers on rubbing;
vigorously;
grey or black with
usually dull and black slight lustre
and appearing fritted
rather than fused
t
May be fissured;
moderate metallic
ring when tapped
on a hard wooden
surface; does not
stain the fingers
on rubbing.
Cross section well
fused and greyish
Gs to Gt
Retains initial volume
Swollen
Examine for degree of swelling
Hard and strong
Slightly swollen
Moderately
swollen
Well fused with a

good metallic ring
when tapped on a
hard wooden
surface
2.8.3
Fischer carbonization assay
Highly swollen
G3 and higher.
Guided by swelling
number, blend with
minimum number
G,
broadly to the crucible swelling number values as shown in

Table 2.4.
Hard, strong
and shrunken
G2
of parts of electrode
carbon to give a
standard G-type
coke
G
*
This test is similar in principle to the Gray-King assay, but

involves a somewhat different apparatus and heating rate. In
one method, the sample is heated in an aluminium retort to
520 C over a period of 80 min. The tars and liquors are
condensed in a water-cooled receiver, while the gas is
allowed to escape into theatmosphere. The liquid and solid
decomposition products are weighed, and the moisture
content of the condensate, as well as that of the original
coal, determined by entrainment with toluene or xylene.
From these data, the percentages of coke, tar and water
given off by the dry coal are determined, and the amount of
gas (plus errors) is calculated by subtraction.
24
Chapter 2
The Fischer assay is most widely used for testing the

response of low rank coals (e.g. brown coal and lignite) to
low temperature carbonization. It is also one of the main
methods used to assess the grade of
25
The Gieseler plastometer is a type of viscometer that

monitors the fluidity of a crushed coal sample as it
undergoes the process of carbonization. This sample is
pressed, under prescribed conditions, around a spindle
equipped with a series of protruding rabble arms pivoted
inside a metal crucible. The crucible is heated from 300 to
600 C at 3C min-1, and torque applied to the spindle by
means of either a pulley and weight arrangement (Fig. 2.14),
or an electromechanical constant-torque device.
The spindle starts to turn as the coal becomes plastic,
and the rate at which it turns, measured in dial divisions per
minute (d.d.m.) is plotted against temperature. The
following data are recorded:
(a) Initial softening temperature
TABLE 2.4 Approximate comparison between crucible swelling
The temperature at which the fluidity exceeds 1.0 d.d.m.

Other values of fluidity may be taken instead of 1.0 d.d.m.
to specify this temperature, but in such cases the value used
must be stated when reporting the plastometer results.
number and other carbonization tests.

(a) Crucible swelling number and Gray-King coke type
(b) Temperature of maximum fluidity
Crucible swelling
number
The temperature at which the fluidity of the coal reaches a

maximum.
Gray-King coke
type
0-%
A-B
1-4
4V2 - 6
C - G2
F - G4
C
O
1
<2
90
m-9
G3 - G,
G7 and above
(c) Maximum fluidity

The maximum degree of fluidity, measured in d.d.m.,
attained by the coal. This may also be reported as the
logarithm (base 10) of that value.
(b) Crucible swelling number and Roga index

Crucible swelling
number
0 - V2
1-2
2Vz - 4
>4
(d) Resolidification temperature

Roga index
0-5
5-20
20 - 45
>45
oil shales. As indicated in Table 2.5, it generally gives a

higher coke yield, for an equivalent coal, than the GrayKing assay at 600 C, and lesser yields of tar, liquor and gas.
2.8.4
Gieseler plastometer
In the process of coke formation, crushed coal passes from a

solid, granular material through a fluid, or plastic state to
become a fused porous solid. The temperature range over
which the coal exists in this fluid state, and the viscosity or
resistance to flow of that fluid are critical factors in the
blending of coals from different sources for large-scale coke
manufacture. These characteristics are tested by the Gieseler
plastometer.
26
Chapter 2
The temperature at which fluidity ceases after passing

through the fluid phase.
TABLE 2.5 Comparison of Gray-King and Fischer carbonization assays. Yields (percentage by weight of dry coal) of carbonization products from
selected Australian coals. Data from Queensland Coal Board (1978) and Edwards (1975). For other analytical data on these samples see Tables
1.19 and 1.20.
Gray-King assay (600 C)
Coal sample location

Millmerran, Qld
Baralaba, Qld
Callide, Qld
Blair Athol, Qld
Goonyella, Qld
Fischer assay
Coke
Tar and oils
Liquor
(%)
(%)
(%)
62.0
94.0
79.3
76.1
20.4
0.2
2.2
86.1
8.0
7.6
0.7
7.0
7.4
1.5
6.6 .
Gas
(%)
Coke
(%)
Tar
(%)
Liquor
(%)
Gas
(%)
10.0
5.1
11.5
9.9
4.4
68.9
96.8
86.9
86.1
8.0
5.1
1.9
3.3
4.1
1.5
8.3
1.2
7.3
82.6
17.7
0.1
2.5
5.1
8.2
4.4

Counter balanced pointer
considerations in the blending of different coals for

commercial coking operations.
The volume changes that occur in carbonization may be
determined by the Audibert-Arnu dilatometer. In this
instrument, the coal is crushed and pressed into a pencil 60
mm long. The sample is then heated, in the absence of air,
from 300 C at a rate of 3C min -1 until the material has
solidified (usually 450-500 C). The length of the pencil is
monitored by means of a piston attached to a recording
device (Fig. 2.15). A graphic plot of length against
temperature is produced, from which the following data are
obtained:
(a) Temperature of initial movement.
(b) Percentage maximum contraction.
(c) Temperature of maximum contraction.
(d) Percentage maximum dilatation (noted as positive or
negative).
(e) Temperature of maximum dilatation.
Fig. 2.14 Operation of the Gieseler plastometer. (From A.S.T.M.

Standard D-1812, 1969.)
(e) Plastic range

The difference between the initial softening temperature
and the resolidification temperature.
The fluidity properties, like other coking
characteristics, depend very heavily on the petrographic
properties of the coal (Section 4.3.6). Coals with a high and
with a low fluidity may be blended to obtain optimum
coking characteristics, but the plastic ranges of the various
components in this case should generally be compatible
with each other (Section 4.3.5). More so than most other
properties, the degree of maximum fluidity is sensitive to
oxidation of the coal, and care must be taken in storage of
samples for such tests.
For equivalent samples, the automatic, constant torque
device generally gives lower values for maximum fluidity
than the manual, pulley operated apparatus. By constrast
the Hoehne plastometer, a similar apparatus that is widely
used in parts of Europe, gives much higher fluidity values
than the Gieseler technique.
2.8.5
(b)
Fig. 2.15 (a) Schematic cross section of an
Audibert-Arnu dilatometer
Audibert-Arnu dilatometer (Berkowitz 1979).
(b) Typical dilatometer curve for a coking coal.
Most coals initially shrink E,

during
carbonization, then swell
softening point; O, contraction point
again as the volatile matter
escapes
and vesicles
are or
(beginning
of porosity).
V, solidification
formed. These volume dilatation
changespoint,
aremaximum
significant
inat which
expansion
phasecan
hardens,
d = dilatation,
determining the amount ofplastic
coal that
be safely
chargedk =
into the coke oven, and arecompression
important (due to softening and melting)
(after Falcon 1978a)
A similar test, but using slightly diffrent techniques is

the Ruhr dilatometer. The coal is pressed in a different way,
and the results generally show less contraction and more
dilatation, for equivalent samples, than do those of the
Audibert-Arnu apparatus.
2.8.6
Roga index
The Roga index is a test that is widely used in Europe to

indicate caking capacity. It is based on pressing a 1 g sample
of the coal, mixed with 5 g of a standard anthracite, and
heating the material, under a relatively small load, at 850 C
for 15 min in a standard crucible. The cohesion of the coke
button produced by this process is then tested in a drum
tumbler, and the Roga index determined from the percentage
of coarse material remaining.
A general correspondence exists between the crucible
swelling number and the Roga index as shown in Table 2.4.
(ii) Tumbler tests tests of coke durability in which a

coke sample of known particle size distribution is tumbled
in a rotating drum under specified conditions, and the
percentage of fines produced is determined. There are
several tests of this type, generally similar in nature, but
each has slightly different specifications and procedures
(Section 4.3.4);
(d)
Metallurgical tests
These are tests of the operating characteristics that the coke

may be expected to have in the blast furnace, such as its
reactivity and strength when hot or after reaction is
complete. Some of these are discussed more fully in Section
4.3.
2.9 MINERAL MATTER IN COAL
(a) Chemical composition
No coal consists entirely of organic compounds. Inorganic

material is also present, either as discrete crystalline solids,
dissolved salts in pore waters, or organometallic compounds
in the coal substance. The term mineral matter is used in
some contexts to cover material of all three types, while in
other usage it is restricted to the crystalline inorganic
constituents or true minerals (in the geological sense)
present in the coal.
It is important, therefore, to distinguish between the
total inorganics and the minerals in the sample. This
especially so in low rank coals where the noncrystalline
forms are particularly abundant (Kiss & King 1979).
Because much of the preceding discussion in this chapter
has treated the total inorganics, however, this section deals
with the special techniques used to evaluate the nature and
significance of the strictly mineralogical component.
Proximate analysis, total sulphur, phosphorus, ash analysis

etc..;
2.9.1
2.8.7
Other tests of coking properties
Most other tests to determine how suitable a coal might be

for coke manufacture, either alone or in a blend, involve the
manufacture of coke from bulk samples in small-scale
replicas of industrial coke ovens. In some cases, a larger
sample may be tested in the actual oven battery for which it
is intended in commercial use.
The coke produced under these conditions is subjected to
a series of tests to determine its composition, strength and
other operational characteristics. The properties that are
determined commonly include:
(b) Physical properties

Size distribution, relative density, porosity etc.;
(c) Strength tests
Tests to determine the strength of the coke, including:
(i) Drop-shatter test a test of coke durability based on
dropping a sample of coke with a particular particle size
distribution, and determining the proportion of fines
produced;
Mode of occurrence of mineral matter
The minerals found in bituminous coals are chiefly silicates,

carbonates, sulphides, sulphates and other species such as
phosphates (Table 2.6). When present in large amounts they
may be seen on a macroscopic scale as bands, lenticles and
nodules in seam exposures, or as fracture fillings and
coatings on joint or cleat surfaces. Further detail can be
obtained by microscopic study, where they may also be seen
as single grains and crystals, or as petrifications or
replacements of the organic components.
A similar range of minerals may also be found in low
rank coals. However, because of the different organic
structure and the greater amount of inherent moisture in
these materials, a large part of the inorganic

TABLE 2.6 Major minerals recognized in coal (Compiled from various sources.)
Silicates:
Clay minerals Kaolinite
Al2Si205(0H)4 Illite
Montmorillonite
Chlorite
Mixed-layer clays
Others Quartz
SiO,
Chalcedony Si02
Feldspar KAlSi308
Tourmaline NaMg3Al6B3Si6027(OH)4
Sulphides Pyrite FeS2
Marcasite FeS2 .
Sphalerite ZnS
Galena PbS
component is also found in non-crystalline form. The exact

nature of these constituents is not always clear, but many
elements probably occur as salts or carboxylic acids dissolved
in the pore water. Some of these may come out of solution
when the coal is dried, forming crystalline impregnations in
the coal and coatings on its exposed surfaces.
2.9.2
Determination of mineral matter
content
The minerals present in coal are of great significance in
aspects of coal classification, testing and use, as well as in
problems such as seam correlation and the development of
depositional models. As pointed out in Section 2.3.4, the ash
represents only the nonvolatile portion of the mineral matter.
Detailed comparison of different coals is therefore best based
on the properties of the mineral-free material, rather than
simply its non-ash components (Section 2.10.2).
A wide range of techniques has been developed for
mineral matter studies. Some are more suited to mineral
identification, while others are directed towards assessment of
the total mineral matter content.
Carbonates Calcite CaC03

Dolomite (CaMg)C03 Siderite
FeC03 Aragonite CaC03
Ankerite {FeMgCa)C03
Dawsonite NaAlC03(0H)2
Strontianite SrC03
Sulphates
Gypsum CaS04. 2H20 Barite BaS04
Anhydrite CaS04 Coquimbite
Fe2(S04)3. 9H20 Szomolnokite
FeS0,H20 Natrojarosite
NaFe3(S04)2(0H)6 Thenardite
Na2S04 Bassanite 2CaS04. H20
Other minerals
Apatite Ca5F(P04)3 Goyazite
SrAl3(P04)2(0H)5H20 Anatase Ti02
Rutile Ti02 Haematite Fe20,
Goethite Fe(OH)3
Zircon ZrSi04
Depending on the purposes of the investigation, they may

include one or more of the following:
(a) Micropetrographic analysis
With the aid of systematic point-counting, micropetrographic
analysis (Section 3.7) may be used to give at least an
indication of the abundance of the major mineral groups
present in a coal sample. The technique is limited, however,
by the difficulty of identifying many species, such as the clay
minerals, from their optical properties alone, and by the
tendency to overlook any minerals finely intergrown with the
organic components. Although it is the principal means by
which the mode of occurrence of various minerals may be
investigated, it does not offer the precision of mineral
identification or quantitative measurement of total mineral
matter content that is available from other methods.
(b) Normative calculation
The total amount of mineral matter can be evaluated from a
series of normative calculations based on the
30
Chapter 2
coals ash content and other chemical properties. Several
The most satisfactory methods for mineral matter
such methods exist, the most comprehensive of which is the
determination, however, are those that remove the organic
King-Maries-Crossley or KMC formula (King et al 1936),
fraction by oxidation, and leave the mineral species,
which estimates the total amount of mineral matter as
essentially unaltered, as a residue. This can be achieved to
follows:
some extent by use of concentrated hydrogen peroxide
(Ward 1974) but difficulties arise with solution of halides,
sulphates and carbonates, either in the peroxide itself or in
MM = 1.13A + 0.8 C02 + 0.5S +2.85 Scn *
pyr
organic acids produced by the oxidation process. Heating of
2.85SAsh + 0.5C1.
the coal for several days in air at around 370 C may also be
where MM = percentage mineral matter, A = percentage used to determine the amount of mineral matter present. The
organic matter is destroyed by the air oxidation, but some
ash, C02 = percentage carbonate C02, Spyr = percentage
minerals, such as expandible clays, sulphates and pyrite also
pyritic sulphur, Ss0i = percentage sulphate sulphur, Cl =
suffer irreversible changes for which allowance must be
percentage chlorine (all in air-dried coal), and
made.
SAsh = (% S03 in ash x 0.40 x % ash)
The most satisfactory technique for determination of
mineral
matter content is the use of an electronically-excited
100
oxygen plasma to destroy the organic matter at a
temperature of around 120 C (Gluskoter 1965). Known as
Other formulae include that of the British Coal
either electronic low temperature ashing (L.T.A.) or radioUtilization Research Association (B.C.U.R.A.), also used in
frequency oxidation (R.F.O.), this method involves dry
the United Kingdom:
oxidation of the coal in an evacuated chamber (Fig. 2.16).
Oxygen, excited to ozone and other species by a radioMM = 1.10A + 0.53S + 0.74 C02 - 0.36
frequency oscillator, is passed around the sample, and
completely removes the organic matter over a period of
and the Parr formula, widely used for American coals:
several days.
Although crystallization of dissolved materials may take
MM = 1.08A + 0.55S
place,
the solid mineral matter is essentially unaffected by
where in both formulae S = percentage total sulphur in airthis
technique.
Only minor dehydration and oxidation
dried coal, and other components are as indicated above.
reactions
normally
occur. For more
As well as the total percentage of mineral matter,
normative methods can also be used to give an estimate of
the relative abundance of each major mineral, or mineral
group, present in the coal and this may be of benefit as an
aid to quantitative interpretation (e.g. Rao & Gluskoter
1973). However, the techniques are based on a number of
assumptions regarding the nature of the mineral species
involved, especially the silicate and carbonate component,
and these may not be true for the coal in question. Normative determinations of the total mineral matter content,
especially by the more simple methods such as the Parr
formula, should also be treated with some caution. The
formula on which the determination is based should also be
stated when giving the results.
(c) Acid digestion
A more direct method of estimating the total amount of
mineral mattter is to dissolve the inorganic components in
hydrochloric and hydrofluoric acids (Radmacher &
Mohrhauer 1956). This leaves the organic fraction of the
coal essentially intact, and allows calculation of the total
percentage of minerals present from the overall loss in
mass. The general nature of these minerals, but not the
actual species involved, can also be determined by chemical
analysis of the acid solutions.
(d) Low-temperature oxidation
31
Fig. 2.16 Principles of radio-frequency oxidation. Oxygen is excited by radio-frequency (R.F.) coil, and passes over coal sample in oxidation
chamber. (From Gluskoter 1965.)
precise studies (Frazer & Belcher 1974), the small amount

of organic carbon remaining in the residue may be
determined separately, and deducted from the mass of
material produced. Prior removal of soluble compounds
may also be included if required.
2.9.3
Mineral identification techniques
As well as providing a relatively precise estimate of the

mineral matter content, low temperature oxidation,
particularly by the radio-frequency method, also provides a
sample suitable for mineralogical analysis. The oxidation
residues can be subjected to further study by X-ray
diffraction (Fig 2.17), the scanning electron microscope,
thermal analysis, infrared spectrometry or other techniques
to identity the actual minerals present and assess their
approximate relative proportions (Russell & Rimmer 1979).
Mineralogical components from combustion, coking,
liquefaction and gasification processes may also be studied
in this way.
Special techniques can be applied, where necessary, to
separate out appropriate fractions such as the heavy
minerals or the clay minerals for detailed analysis. Chemical
data on the coal, such as the pyritic sulphur and carbonate
C02 contents, can also be used to help assess the relative
proportions of the minerals identified by these techniques.
Such analysis is also possible, at least for coals with a
high ash or mineral matter content, by applying many of
these techniques directly to the coal itself. The organic
materials are essentially non-crystalline, and thus an X-ray
diffractogram of coal consists almost entirely of peaks
representing the mineral components (Rekus & Haberkorn
1966). The strongly exothermic reactions of coal
combustion may also be suppressed in differential thermal
analysis by use of an inert nitrogen atmosphere again
allowing peaks due to any particularly abundant mineral
species to be identified (Warne 1964).
2.9.4
Minerals present in coals
Depending on the nature of the coal sample involved, the

mineral matter present may be derived from a number of
different sources. Bulk samples taken from the coal as
mined, for example, normally contain mineralogical
contaminants due to the presence of intra-seam bands of

non-coal material, as well as possibly debris from the
adjacent roof and floor strata. However, individually
selected specimens, or plies and seam composites free of
these materials, usually contain a distinctive suite of
minerals dominated by those listed in Table 2.6.
32
Chapter 2
Fig. 2.17 Typical X-ray difFractograms of R.F.O. residues, (a) Illinois Basin, U.S.A. (b) Sydney Basin, Australia, (c) Maryborough Basin, Australia,
Ap, apatite; Cq, coquimbite; Ct, calcite; Q, quartz; D, dolomite; E, expandible lattice clay minerals; Sd, siderite; I, illite; K, kaolinite; P, pyrite;
Sz, szmolnockite.
(a) Quartz
Quartz is common in most coals, but seldom as a major
constituent. It often occurs as angular grains in clay-rich
bands, suggesting a detrital origin. However, it may also
occur as a chemical precipitate, possibly originally in the
form of chalcedony, infilling cell cavities in the coal
macerals or as veins cutting across the coal structure.
(b) Kaolinite
Although often a minor constituent or even completely

absent from the associated non-coal lutites, kaolinite is
found in a large number of bituminous coals. It is usually
very well crystallized and in some cases is the only clay
mineral that can be identified even by detailed X-ray
diffraction. Some of it may occur as petrifactions or cellcavity infillings, suggesting an authigenic origin in the
original peat. The mineral also occurs as bands, pellets or
vermicular aggregates, and as an infilling of cleat fractures.
The origin of this material is discussed by Rao and
Gluskoter (1973), Ward (1977, 1978), and Gaigher (1980).
(c) Other clay minerals
precipitation from groundwater.
Well crystallized illite is a common constituent of coal from
some areas, but may be completely absent in others.
Montmorillonite, chlorite and regular to irregular mixedlayer clay minerals are also found in many coals throughout
the world. The assemblage of these is usually similar, but not
identical to that found in the associated non-coal lutites. It is
likely that they mostly represent detrital contaminants of the

original peat, modified to a variable extent by early or late
diagenetic processes.
(d) Sulphide minerals

(a) Storage and handling
Pyrite is a common constituent of many coals, particularly

those closely associated with marine strata, Together with
small amounts of sphalerite, marcasite, galena and other
species, it occurs as lenticular masses, euhedral crystals,
framboidal aggregates, cell infillings, as veins and on cleat
surfaces. These minerals probably represent the result of
bacterial reduction of sulphate-rich peat waters during early
diagenesis (Rao & Gluskoter 1973), but later remobilization
is also likely in some cases as well.
(e) Carbonate minerals
The carbonate minerals found in most bituminous coals are

siderite, calcite and dolomite or ankerite. Siderite commonly
occurs as spheroidal nodules within the coal, and was
apparently formed by chemical precipitation during early
diagenesis. It is most abundant in coals with a low pyrite
content, and probably represents the interaction of iron with
dissolved C02 in peat waters where sulphate concentrations
were too low for pyrite production. Calcite, dolomite and
ankerite are mostly late-stage accumulations in bituminous
coals, occurring as veins and on cleat surfaces.
(f)
Sulphate minerals
Most of the sulphate minerals found in coal owe their origin

to oxidation of pyrite. Hydrous iron sulphates such as
coquimbite and jarosite are formed in this way. They can be
readily seen as crystalline deposits on exposed faces and as
cleat infillings in outcrops, mines and masses of broken coal.
Where calcite is present, the acids produced from pyrite
oxidation may react with it to form gypsum, which may in
turn be dehydrated to bassanite or anhydrite during radiofrequency oxidation. In arid areas, however, gypsum may
also form as veins in near-surface coal seams by
(g) Other minerals
Most of the other minerals in bituminous coals are relatively
minor accessories. Apatite is among the most common,
occurring as ptrifications in the coals organic components
(Cook 1962), while in a few coals, aluminophosphate
minerals of the goyazite group are also found (Ward 1974).
Feldspar is present in some coals, apparently as a detrital
constituent, and minor amounts of other minerals are
sometimes noted during petrographic examination (e.g.
Kemezys & Taylor 1964).
2.9.5
Significance of the mineral matter
Mineral matter forms a significant part of nearly all coals,

and must be considered in assessing a particular deposit for
utilization. It can have an effect on the coals behaviour at
low temperature (e.g. during storage), at medium
temperature, such as in carbonization, and at the high
temperatures of the combustion process. Knowledge of the
amount and composition of the mineral matter is also
important for many types of coal classification.
33
One of the most important problems in the handling of many

coals is the generation of acid conditions in the mine or
washery waters by pyrite oxidation. This leads to corrosion
of mining and preparation equipment, as well as to pollution
control problems when the waters are discharged to the
environment. Acid runoff may also be developed from
exposed stockpiles of coal, or from refuse and overburden
materials, which are often more enriched in pyrite than the
coal itself.
Problems of a different kind are generated by the
presence of abundant swelling clays, such as montmorillonite, in the coal or its associated beds. As indicated
in Section 2.6.4, this material disperses readily in the water
used for coal preparation, altering its density and forming a
high-ash film on the clean coal particles. Once dispersed, it
is very difficult to remove from the water before it is
recycled through the preparation plant.
Coals and associated materials rich in montmorillonite
are also subject to swelling and shrinking with changes in
humidity. When exposed in stockpiles etc. this may combine
with the natural tendency, at least in low-rank coals, for the
organic matter to develop shrinkage cracks, causing the
material to disintegrate and form an undesirable excess of
fine particles in the broken coal mass. Such swelling clays
can also make stockpiles and refuse embankments subject to
slope stability problems.
Coarse particles of hard minerals, such as quartz, can
also lead to abnormal abrasion and wear on the pulverizing
equipment used for many combustion and liquefaction
processes (Section 2.7.4). This can affect the cost or design
of a coal-using plant, or the marketability of one coal in
relation to another when a choice is available.
(b) Combustion
When the coal is burned, most of the mineral structures are
broken up and new species are formed (OGorman & Walker
1973). Volatile components such as chlorine from dissolved
salts, may foul or corrode the boiler surfaces, or escape with
the stack gases as pollutants. Where pyrite is abundant,
special treatment of these gases may be necessary to remove
the S02 produced (Section 4.2.4).
The fusion temperatures of the ash also depend largely
on the nature of the mineral matter. Coals rich in kaolinite
have high ash fusion temperatures (Ward 1978), while in
those with abundant montmorillonite, chlorite etc., the ash
fuses at significantly lower temperatures and clinkering may
result. Low ash fusion temperatures are likewise produced
by the fluxing action of carbonates, sulphates and pyrite,
even if the coal has a large proportion of otherwise
refractory clay minerals (Huffman et a! 1981).
(c)
Carbonization and liquefaction
The minerals present in a coal are not altered to the same

extent by coking and liquefaction processes as they are by
34
Chapter 2
combustion. The minerals may affect the cokes strength or (b) Air-dried
reactivity, and their composition must be considered when
The data are expressed as percentages of the air-dried coal,
determining the blend of iron ore, limestone and coke
including inherent, but not adventitious moisture.
required in the blast furnace for efficient metallurgical
conditions (Brown et al 1964). Minerals may take part in
many liquefaction processes, acting as catalysts in some
cases to increase the yield of hydrocarbon products, and in
other as inhibitors, poisoning the synthetic catalysts used
(Russell & Rimmer 1979). In addition, volatile components
of the mineral matter may contaminate the liquefaction
products, or form a coating on critical parts of the process
equipment used.
(d) Coal classification
Meaningful comparison of the organic components of
different coals is only possible if allowance is made for
dilution by the moisture and the mineralogical constituents.
Evaluation of the dry, mineral-matter free composition of the
coal (Section 2.10.1) is only possible when the proportion of
mineral matter has been determined either by normative
calculation, acid solution or radio-frequency oxidation
techniques. Quantitative knowledge of the minerals present,
their composition and dehydration characteristics (e.g. by
chemical and thermogravimetric analysis of the oxidation
residues) can then be used to allow for their contribution to
the amounts of carbon, hydrogen and volatile matter
originally determined in the air-dried coal.
2.10
REPORTING OF COAL ANALYSES
2.10.1
Basis of analytical data
Most analyses of coals are carried out on air-dried samples,

and the percentages of the various constituents calculated in
proportion to the mass of that material. For many purposes,
however, this value is of little significance. In commercial
operations, a certain amount of adventitious moisture forms
part of the coal that is mined, shipped, and delivered to the
consumer. The percentage of (say) ash in relation to the total
mass of coal supplied in such cases is more meaningful than
the percentage in relation to a state that is never attained in
practice.
On the other hand, comparison and classification of coals
is based essentially on the nature of the organic fraction. It is
necessary to allow for the effects on chemical composition
and other properties brought about by mineral impurities in
order to make use of such classifications, and thus the
percentages may need to be re-expressed as part of a pure
coal rather than of a moist, mineral-bearing material.
In both these situations, the analytical results can be
modified by appropriate corrections to allow expressions on
a different basis. The most commonly used bases for
reporting of analytical results are indicated in Figure 2.18:
(a)
As received or as sampled
The data are expressed as percentages of the coal including

the total moisture content.

35
(c) AVM = 0.13A + 0.2Spyr + 0.7CO2 + 0.6C1 - 0.2
Dr
y
where AVM = reduction in the percentage of volatile matter
or
(air-dried) to allow for mineral-induced volatiles, A =
percentage ash in the coal (air-dried), Spyr = percentage
pyritic sulphur in the coal (air-dried), C0 2 = percentage
carbonate C02 in the coal (air-dried), Cl = percentage
chlorine in the coal (air-dried).
Surface moisture
Inherent moisture
Ash
Volatile
mineral
matter
Pure
coal
%VMdmmr = 100 x (%VMairdried - AVM)

0
0
Fixed
carbon
0
e
<0
to
0
100 % moisture % mineral matter

As received
Volatile
organic
matter
Volatile
matter
Air dried
The percentage of volatile matter, on a dry, mineralmatter free basis, is therefore given by:
Dry
Mineral
matter
Dry, ash free
Total
moistur
e
C
E
>
Q
Fig. 2.18 Components of a coal included when reporting

analyses to different bases.
moisture free
The data are expressed as percentages of the coal after the
inherent moisture has been removed.
(d) Dry, ash-free (d.a.f.)
The coal is considered, in proximate analysis, to consist only
of volatile matter and fixed carbon, on the basis of
recalculation with ash and moisture removed. This is the
simplest way to compare the organic fractions of coals
without the diluting effects of inorganic components.
However, it does not allow for the volatile matter derived
from the minerals present in air-dried coals.
(e)
Dry, mineral matter-free (d.m.m.f.)
The coal is also considered to consist solely of volatile

matter and fixed carbon, but it is necessary that the total
amount of mineral matter rather than ash be determined.
This may be done either directly or indirectly, as indicated in
Section 2.9.2.
Allowance is also made in dry, mineral matter-free data,
for the contribution to the air-dried volatile matter that
comes from the mineral components. This may also be done
directly, on a sample of the mineral matter isolated by R.F.O.
techniques, or indirectly, by the following formula:
The percentage of fixed carbon is given by the

difference between this value and 100%.
Conversion of analytical data to any other basis is
achieved by multiplying the given result by a factor as
shown in Table 2.7.
2.10.2
Coal classification
For most geological purposes, the rank and type of the coal,
as determined by petrographic methods (Section 3.6.3),
provide an adequate basis for the comparison of different
materials. However, in industrial usage of coal, many of the
chemical parameters are more significant, and a number of
schemes have been drawn up to classify coals for academic
and industrial purposes.
(a) Seylers classification
Seylers classification scheme, outlined in 1933, is still
widely used today. It is based on the percentage of carbon
and hydrogen present in the coal, calculated to a dry,
mineral-matter free basis, as shown in Fig. 2.19. Alternative
criteria, shown by other axes superimposed on these, are the
percentage of volatile matter and the calorific value (specific
energy), both also on a d.m.m.f. basis.
Most coals plot on the curved band indicated in Fig.
2.19. Low rank coals have higher hydrogen and lower
carbon contents than high rank coals, and plot to the right of
the graph. At the other end of the scale, anthracites, with
almost no hydrogen present, plot in the lower left-hand
sector. Variations in coal type are expressed, to some extent,
by use of the terms per- hydrous for hydrogen-rich material
and sub-hydrous for hydrogen-poor samples. A series of
such prefixes, in conjunction with the term appropriate for
the rank
36
Chapter 2
TABLE 2.7 Formulas for calculation of results to different bases* (after correction for changes during analysis) (From British Standard 1016, Part
16, 1971.)
Wanted result
Given result
As analysed (air dry)
As sampled (as received)

(as despatched) (as fired)
As analysed
100 - Mas
(air dry)
100 - Mad
As sampled (as
received)
Dry
Dry, ash free
100
100
100 - Mad
100 - (Mad + Aad)
100
100 - (Mad +MMad)
100 - Mad
100
(as despatched) (as

fired)
100 - Mas
100 - Mas
Dry
100 - Mad
100 - Mas
100
100
100
100
100 - Ad
100 - MMd
Dry, ash free
100 (Ma(j + Aad)

100
Dry, mineral
matter free
100 - (Mad + MMad)

100
100 - (Mas + Aas)

100
100 - (Mas + MMas)
100
100
Dry,
mineral matter free
100 - (Mas + Aas)
100
100 - (M + MM )
' as as7
100 - Ad
100 - Ad
100
100 - MMd
100 - MMd
100
100 - MMd
100 - Ad
*Use of the above formulas alone is not sufficient when calculating volatile matter to different bases.
of the coal, is used to classify the material fully (Table
2.8).
(b) A.S.T.M. classification

The classification of coals published by the American
Society for Testing and Materials (A.S.T.M. D388-77) is
used extensively in North America and many other parts of
the world. It is based on two fundamental properties of
practical significance, the fixed carbon (and hence the
volatile matter) content and the calorific value (or specific
energy). Further classification for some coals is then based
on their agglomerating or coking properties, expressed by
the nature of the residue after determination of the volatile
matter content.
Coal that has a fixed carbon content of 69% or more
(d.m.m.f. basis) is classified according to the value of that
property as shown in Table 2.9. If the coal has a fixed carbon
content below 69%, classification is based on a combination
of its calorific value and its agglomerating characteristics.
Although claimed to represent a classification by rank,

coals with different type, even if of equivalent rank, may still
be grouped into different classes because of their different
physical and chemical properties. A dull bituminous coal
with a low volatile content (d.m.m.f.) may appear from this
classification to have a higher rank than a ply of bright coal
from the same seam. Coals with particularly
unusualproperties, such as the non-banded, volatile rich
sapropelic coals (Section 3.2.2) are specifically excluded
from the A.S.T.M. classification.
(c) International coal classification
Devised by the United Nations Economic Commission for
Europe to assist international trade, and subsequently
approved by the International Organization for
Standardization (I.S.O.), this classification system uses a
series of numbers to give a general summary of the
37
Fig. 2.19 Seylers classification of coal. (Modified from Francis 1961.) All results are given on a dry, mineral free basis (Parr formula).
o
oo
TABLE 2.8 Parameters used in Seylers coal classification.
Class (% C)
H
(%)
Anthracite
Carbonaceous
(>93.03)
(93.3-91.2)
Pseudo-bitumin-
Meta(91.2-89.0)
Genus
Per-bituminous
>5.8
Bituminous
5-5.8
Semi-bituminous
Carbonaceous
Anthracitic
Per-bituminous
(per-metabituminous)
Meta-bituminous
Bituminous
Ortho(89.0-87.0)
Para(87.0-84.0)
Per-bituminous
(per-orthobituminous)
Ortho-bituminous
Per-bituminous
(per-parabituminous)
Para-bituminous
ous species
Semi-bituminous
Sub-bituminous
Sub-bituminous
4.0-4.5
Semi-anthracitic
species (orthosemi-bituminous)
Carbonaceous
(sub-metabituminous)
Pseudo-carbona-
(sub-orthobituminous)
Pseudo-carbona-
Pseudo-carbona-
<4
species
Dry steam coal
Ortho-anthracite
species (orthocarbonaceous)
Pseudo-anthra-
ceous (sub-metabituminous)
Pseudo-anthra-
ceous (sub-orthobituminous)
Pseudo-anthra-
ceous (sub-parabituminous)
Pseudo-anthra-
True anthracite
cite (subcarbonaceous)
cite (sub-metabituminous)
cite (sub-orthobituminous)
cite (sub-parabituminous)
4.5-5.0
Sub-bituminous
Lignitous MetaOrtho- (84-85) (8075)

Per-lignitous
Lignitous
Meta Ortho C
Sub-lignitousha
pt
Meta Ortho er
Class
I. Anthracitic
II. Bituminous
Group
Abbreviation
1. Meta-anthracite
2. Anthracite
3. Semi-anthracite^:
ma
an
$a
IV. Lignitic
Volatile matter
limits
(% d.m.m.f.)
(% d.m.m.f.)
Equal to
or greater
than
98
92
Less
than
86
98
92
Greater
than
Equal to or
less
than
2
8
14
1. Low volatile
bituminous coal
2. Medium volatile
lvb
78
86
14
22
bituminous coal
mvb
69
78
22
31
3. High volatile A
bituminous coal
4. High volatile B
hvAb
69
31
bituminous coal
5. High volatile C
bituminous coal
III. Sub-bituminous
Fixed carbon
limits
1. Sub-bituminous A
coal
2. Sub-bituminous B
hvBb
hvCb
Calorific value limits

(Btu lb
Equal to or
greater
than
Agglomerating
m.m.m.f.f)
character
Less
than
> nonagglomerating
>
, commonly
agglomerating H
14 000
13 000
14 000
f 11 500
13 000
\ 10 500
11 500
>
subA
10 500
11 500 X
coal
3, Sub-bituminous C
coal
subB
9 500
10 500
subC
8 300
9 500
1, Lignite A
2. Lignite B
ligA
ligB
6 300
8 300
6 300
agglomerating
Ch
em
ica
l
An
aly
sis
an
d
Cl
as
sif
ica
tio
n
of
Co
al
non-agglomerating
>
O
N
'O
39

coals chemical and physical characteristics. The properties
chosen are those that reflect the usefulness of the coal in its
principal market areas, namely for coke production and
steam-raising applications, and as a result the classification
is widely used in many assessments of coal for industrial
purposes.
In this classification, each coal is described by a threefigure number. For 'hard coals, with a specific energy of
more than 23.86 MJ kg-1 (moist, ash free), these digits are
derived as follows:
2nd digit (coal group)
1st digit (coal class)
2.10. ,
This is based on the amount of volatile matter in the

coal, on a dry, ash free basis. Where the coal has less than
33% volatiles, however, the gross specific energy (moist,
ash free basis) is used instead.
TABLE
This is based on the free swelling index of the coal, or

alternatively its Roga index.
3rd digit (coal sub-group)

This is based on the Gray-King coke type of the coal, or
alternatively its behaviour in the Arnu-Audibert
dilatometer.
The actual numbers used are summarized in Table
For soft coals with a specific energy of less than 23.86
MJ kg-1 (moist, ash free) the classification is based on a
four figure code as follows:
2.10 International classification of hard coals. (After Williamson 1967.)

Value
Volatile matter (dry, ash free %)
Gross specific energy (Moist, ashfree*) (MJ kg"1)
1st digit
0-3
(coal class)
1A
IB
2
3A
3B
4
5
6
TABLE 2.11 International classification of sott
' 7 coals (i.e. coals with a gross
specific energy below 23.87 MJ kg * (After Williamson
1967).
8
Value
Total moisture
content of freshly
9
mined coal (ash free)
(%)
1st and 2nd digits
10
(class
parameter)
2nd
digit
11
12
13
14
15
(coal group)
Value
0
1
2
4
<20
20-30
30-40
40-50
50-60
60-70
Tar yield (d.a.f.)

Value
Value
3rd digit
3rd and 4th digits
(coal
(group number)
sub-group)
0
00
1
2
3
4
5
10
20
30
40
(%)
<10
10-15 ;
15-20
20-25
>25
* Moist, ash-free basis at 30 C; 96% relative humidity.

* at 30 C; 96% relative humidity, t For information only.
1st and 2nd digits (class number)

This is based on the total moisture content of the ash
free coal.
3rd and 4th digits (group
number)
This is based
on the
tar yield (d.a.f.) in low
temperature carbonization.
>3-6.5
>6.5-10
>10-14
>14-16
>16-20
>20-28
>28-33
. >33-41J .
> 33-44J
>35-50f
> 42-50J
>32.45
32.45-30.15
30.15-25.55
25.55-23.87
Free swelling index

(crucible swelling no.)
Roga index
0-V2
0-5
>5-20
>20-45
>45
1-2
2V2-4
>4
Dilatometer .
max. dilation (%)
Gray-King coke type

A
B-D
E-G
G.-G.
G
5-G8
>G8
non-softening
contraction only
<0
>0-50
. > 140
>50-140
40
Chapter 2
(d) Australian standard coal classification

The method used for classification of Australian hard coals
(those with a specific energy greater than 27.08 MJ kg 1) is
described in Australian Standard 2096-1977. Like the
international classification mentioned above, it summarizes
the coals properties by means of a multi-digit number.
Each digit in the sequence represents a particular coal
property as follows:
1st digit (coal class)
This is based on volatile matter (d.m.m.f. basis) for coals
with less than 33% volatile matter, or on gross specific
energy (d.a.f. basis) for other coals.
2nd digit (coal group)
This is based on the crucible swelling number of the coal.
3rd digit (coal sub-group)
This is based on the Gray-King coke type exhibited by the
coal.
4th digit (ash number)
This is based on the ash content (dry basis) of the coal. This
digit is given as a qualifier in brackets.
The Australian classification allows a more
comprehensive specification than many others of similar
form, by incorporating the coals ash content into the
designation given. This is important as many coals from
that region have high ash contents, compared to similar
European or American products. A summary of the values
on which the various components of the classification are
based is given in Table 2.12.
(e) National Coal Board classification
The classification derived by the National Coal Board of
the United Kingdom uses a three-figure numerical code to
TABLE 2.12 Australian standard classification of hard coal. (From
Australian Standard 2096-1977)
Value
1st digit
(coal class)
2nd digit
(coal group)
(continued on p. 2)
Volatile matter
(d.m.m.f.)
(%)
Gross specific
energy (d.a.f.)
(MJ kg1)
1
2
3
slO.O
10.1-14.0
14.1-20.0
4A
4B
20.1-24.0
24.1-28.0
5
6
7
8
9
28.1-33.0
33-41*
>33.82
33-44*
35-50*
42-50*
32.02-33.82
28.43-32.02
27.08-28.42
Value
Crucible swelling no.
0
1
2
3
4
O-V2
1-2
2V2-4
4V2-6
6V2-9
classify bituminous coals and anthracites on the basis of

their volatile content and coking properties. The first two
digits of the classification are based on the amount of
volatile matter in the coal, expressed on a dry, mineralmatter free basis, and the
41

TABLE 2.12 Australian standard classification on hard coal. (From
Australian Standard 2096 1977). (continued from p.71)
3rd digit
(coal sub-group)
4th digit
(ash number)
Value
Gray-King coke type
0
1
2
3
4
5
A
B-D
E-G
GpG,
G5-G8
G,"
Value
Ash (dry basis) (%)
(0)
(1)
^4.0
4.1-8.0
(2)
8.1-12.0
(3)
(4)
(5)
(6)
(7)
(8)
12.1-16.0
16.1-20.0
20.1-24.0 ,
24.1-28.0
28.1-32.0
>32.0
third digit on the Gray-King coke type as illustrated in

Table 2.13.
Coals with less than 19.6% volatile matter (d.m.m.f.)
are classified by this parameter alone (main classes 100 and
200), and the Gray-King values shown in the table are for
information only. If the coal has high ash content (greater
than 10%) it must be cleaned by a float-sink or similar
process prior to analysis, giving the maximum yield of coal
with an ash content of 10% or less. Coals that have been affected by igneous intrusions (heat-altered coals) are further
designated by the suffix H after their numerical
classification (e.g. 102H; 301aH), while those that are
oxidized or weathered are designated by adding the letter W
(e.g. 701W).
Some examples of these different coal classification
schemes, using a range of Australian bituminous coals, are
given in Table 2.14.
* Values for information only.
2.13 Coal classification system used by the National Coa Board. (After Williamson 1967.)
Volatile matter
Coal rank code
(d.m.m.f.)
Gray-King coke type
(%)
Class
Sub-class
Main class(es)
Under 9.1
100
TABLE
<6.1
6.1- 9.0
101
102
200
A-C*
9.1-11.5
11.6-13.5
A-B*
B-C*
f Dry steam coals
13.6-15.0
B-G*
15.1-17.0
17.1-19.5
E-G4*
G1-G8*
19.6-32.0
19.6-32.0
19.6-27.5
27.6-32.0
G4 and over
|G4 and over
;
302
19.6-32.0
G-G3
303
19.6-32.0
A-G
201a
201b
202
203
204
300
301
301a
301b
400-900
(continued on p. 73)
"j
A* ' k Anthracitef
9.1-19.5
9.1-13.5
201
400
General description
.
Over 32.0
Low volatile steam coal
J
1
> Coking steam coals
Medium volatile coals

\
>Pnme coking coals
Medium volatile medium-caking or

weakly caking coals
Medium volatile, weakly caking to
non-caking coals
High volatile coals
TABLE 2.13 Coal classification system used by the National Coal Board. (After Williamson 1967.) (continuedfrom p. 72)
Coal rank
code Main class(es)
500
600
700
800
900
Gray-King coke
type
Volatile matter
(d.m.m.f.) (%)
Class
General
description
Sub-class
401
402
32.1-36.0 3
Over 36.0 /
G9 and over
501
502
32.1-36.0 'l Over 36.0 /
601
602
High volatile, very strongly caking coals

G5-G8
High volatile, strongly caking coals
32,1-36.0 3 Over 36 f
G1-G4
High volatile, medium caking coals
701
702
32.1-36.0 ) Over 36.0 /
E-G
High volatile, weakly caking coals
801
802
32.1-36.0 > Over 36.0

J
. C-D
901
902
32.1-36.0 ) Over 36.0 J
A-B
High volatile, very weakly caking coals

High volatile, non-caking coals
f It is sometimes more convenient to use a hydrogen content of 3.35% (d.m.m.f.) rather than the volatile content of 6.1% to distinguish
between classes 101 and 102. *
For information only.
TABLE
2.14 Examples of coal classification for some Australian coals.
Blackwater
Qld
Locality
Goonyella
Qld
Lithgow
N.S.W.
Volatile matter (d.m.m.f) (%)
Maximum dilation (%)
(d.a.f.) (%)
Gross specific energy (d.a.f.) (MJ kg-1) (m.a.f.) (MJ kg-1) Crucible
swelling number Gray-King coke type Roga index
Ash (dry basis) (%)
.
International classification A.S.T.M. classification Australian Standard

classification N.C.B. classification
29.6
30.2
27.4
. 37.9
38.6
28.0
36.38
35.32
34.87
33.84
8
G5
2
C
69
8.2
-25
84
7.8
77
35
11.2
-31
532
mvb
532 (2)
305
434
mvb
4B44 (1)
301B
611
hvAb
611 (2)
800
(meditan
volatile,
(medium
volatile,
(high
volatile,
medium
caking)
strong
caking)
35.64
33.79
5>/2
very weakly
caking)

2 Chemical Analysis and Classification of Coal

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2 Chemical Analysis and Classification of Coal

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2 Chemical analysis and classification of coal

Classes of coal analysis

An account of the various organic compounds actually

This gives the relative amounts of light organic compounds

This determines the total amounts of each of the principal

properties. These tests may be regarded as miscellaneous

The methods of sample collection and laboratory testing for

SAMPLING FOR COAL ANALYSIS

Even the most precise analytical determination is useless for

drill cores or cuttings, and from masses of broken coal such

Sampling a coal face

An in situ exposure of a coal seam in a mine or outcrop is

(b) Strip or channel sampling

Sampling coal by drilling

The methods used in exploratory drilling of coal seams are

Sampling of broken coal

Chemical Analysis and Classification of Coal

Fig. 2.2 Segregation of particles in a simple stockpile.

In a mass of broken coal, such as a stockpile, the particles

Once transported to the laboratory, the methods of sample

The core is generally transported to the laboratory with as

Bulk sample from

Determine particle size

Crush and analyse

Each density fraction

Crush and analyse

Product and tailings

Crush and analyse [ Combine as required to form

Crush and analyse

Reconstituted clean-coal products Reconstituted refuse materials

Chemical Analysis and Classification of Coal

Almost all analysis requires the coal to be air-dried.

As indicated in Section 2.1, proximate analysis gives a

f------Each coal ply

Combine with other

Combine with other noncoal plies to form

Each non-coal ply

X-radiography Detailed logging

Combine with appropriate other fractions to form Reserve

- Shale breakdown testing

Further testing and analysis

Reconstituted refuse material

Further testing and analysis

The moisture in a coal may occur in four possible forms:

This is extraneous water held as films on the surface of the

This is water incorporated in some of the coals organic

Chemical Analysis and Classification of Coal

process is required to prevent fixation of sulphur in the ash.

The fixed carbon content of a coal is the carbon found in the

2.4 ULTIMATE ANALYSIS

Carbon, hydrogen and oxygen are of great commercial

Carbon and hydrogen

Carbon and hydrogen occur mainly as complex hydrocarbon

The nitrogen found in coals appears to be mainly confined to

Chemical Analysis and Classification of Coal

(b) X-ray fluorescence or similar analysis, under

Oxygen is a component of many of the organic compounds

2.5 MISCELLANEOUS CHEMICAL ANALYSES

samples. Some of these tests are used to enable correction of

Although the total sulphur content provides sufficient data

Carbonate carbon dioxide

Carbonate minerals, principally calcite, dolomite, ankerite

content assists in calculation of the mineral matter content