TESTING OF MATERIALS

COAL & COKE TESTING

Content
Proximate test
Ultimate analysis
Sizing
MICUM TEST
CRI
CSR.
Analysis of Coal
In order to assess the quality of coal the following two types of analysis are
made.

1. Proximate Analysis It includes the determination of moisture, volatile

matter, ash and fixed carbon. This gives quick and valuable information
regarding commercial classification and determination of suitability for a
particular industrial use.

2. Ultimate Analysis It includes the determination of carbon, hydrogen, nitro-

gen, sulphur and oxygen in coal. Since it is used
For the determination of elements present in the coal, it is also called
elemental analysis. This analysis gives exact results and are useful in
calculating the calorific value of coal using Dulong's formula.
Proximate analysis
(1) Moisture: About 1 g of finely powered air-dried coal sample is weighed in a
crucible. The crucible is placed inside an electric hot air-oven, maintained at 105° -
110°C. The crucible is allowed to remain in oven for 1 hour and then taken out,
cooled in a desiccator and weighed. Loss in weight is reported as moisture (on
percentage-basis).

Loss in weight x 100

Percentage of moisture =
Wt. of coal taken
(2) Volatile matter: The dried sample of coal left in the crucible in (1) is then
covered with a lid and placed in an electric furnace (muffle furnace), maintained at
925°± 20°C. The crucible is taken out of the oven after 7 minutes of heating. The
crucible is cooled first in air, then inside a desiccator and weighed again. Loss in
weight is reported as volatile matter on percentage-basis.
Loss in weight due to removal of volatile matter x 100
Percentage of volatile matter =
Wt. of coal sample taken
(3) Ash: The residual coal in the crucible in (2) is then heated without lid in a muffle
furnace at 700 ± 50° C for 1/2 hour. The crucible is then taken out, cooled first in air,
then in desiccator and weighed.

Heating, cooling and weighing is repeated, till a constant weight is obtained. The
residue is reported as ash on percentage-basis.

Percentage of ash = Wt. of ash left x 100

Wt. of coal taken

(4) Fixed carbon: Percentage of fixed carbon = 100 - % of (moisture + volatile matter
+ ash) high percentage of rued carbon is desirable.
Importance of proximate analysis
Proximate analysis provides following valuable informations in assessing the
quality of coal:

(1) Moisture: Moisture lowers the effective calorific value of coal. Moreover,
it quenches the fire in the furnace. Hence, lesser the moisture content,
better the quality of coal as a fuel. However, presence of moisture, up to
10%, produces a more uniform fuel-bed and less of "fly-ash".

(2) Volatile matter: A high volatile matter containing coal burns with a long
flame, high smoke and has low calorific value. Hence, lesser the volatile
matter, better the rank of the coal. Higher volatile content in coal is
undesirable.
A high volatile matter content means that high-proportion of fuel will be distilled and
burned as a gas or vapour. The volatile matter present in the coal may be combustible
gases (such as methane, hydrogen, carbon monoxide and other hydrocarbons) or non-
combustible gases (like CO2 and N2). Volatile matter content is of special significance in
coal gas manufacture and in carbonization plants, particularly when by-product recovery is
the main object. Thus, high-volatile matter containing coals do not cake well; whereas
medium-volatile matter content coals are capable of yielding hard and strong coke on
carbonization.

(3) Ash is a useless, non-combustible matter, which reduces the calorific value of coal.
Moreover, ash causes the hindrance to the flow of air and heat, thereby lowering the
temperature. Also, it often causes. trouble during firing by forming clinker), which block the
inters paces of the grate. This in-turn causes obstruction to air supply; thereby the burning
of coal becomes irregular. Hence, lower the ash content, better the quality of coal. The
presence of ash also increases transporting, handling and storage costs. The presence of
ash also causes early wear of furnace walls, burning of apparatus and feeding mechanism.

(4) Fixed carbon: Higher the percentage of fixed carbon, greater is its calorific and better
the quality coal. Greater the percentage of fixed carbon, smaller is the percentage of
volatile matter. This also represents the quantity of carbon (in coal) that can be burnt by a
primary current of air drawn through the hot bed of a fuel.
Ultimate analysis
Carbon and hydrogen: About 1-2 g of accurately weighed coal sample is
burnt in a current of oxygen in a combustion apparatus. C and H of the coal
are converted into CO2 and H2O respectively. The gaseous products of
combustion are absorbed respectively in KOH and CaCl2 tubes of known
weights. The increase in weights of these are then determined.

Increase in weight of KOH tube x 12 x 100

Percentage of C = Weight of coal sample taken x 44

Increase in weight of CaCl2 tube x 2 x 100

Percentage of H = Weight of coal sample taken x 18
Significance of ultimate analysis

(1) Carbon and hydrogen: Greater the percentage of carbon and hydrogen
better is the coal in quality and calorific value. However, hydrogen is mostly
associated with the volatile matter and hence, it affects the use to which the
coal is put. Also higher percentage of carbon in coal reduces the size of
combustion chamber required. The amount of carbon, the major
combustible consti1fent of coal, depends on the type of coal and its
percentage increases with rank from lignite to anthracite. Thus, percentage
of carbon forms the basis of classification of coal.

(2) Nitrogen has no calorific value and hence, its presence in coal is
undesirable; thus, a good quality coal should have very little nitrogen
content.
Nitrogen: About 1 g of accurately weighed powdered 'coal is heated with concentrated H2SO4
along-with K2S04(catalyst) in a long-necked flask(called Kjeldahl's flask). After the solution becomes
clear, it is treated with excess of KOH and the liberated ammonia is distilled over and absorbed in a
known volume of standard acid solution. The unused acid is then determined by back titration with
standard NaOH solution. From the volume of acid used by ammonia liberated, the percentage of N
in coal is calculated as follows:
Volume of acid used x Normality x 1.4
Percentage of N = Weight of coal taken

Sulphur is determined from the washings obtained from the known mass of coal, used in a bomb
calorimeter for determination of a calorific value. During this determination, S is converted into
sulphate. The washings are treated with barium chloride solution, when barium sulphate is
precipitated. This precipitate is filtered, washed and heated to constant weight.

Weight of BaSO4 obtained x 32 x 100

Percentage of S = Weight of coal sample taken in bomb x 233

Ash determination is carried out as in proximate analysis.

Oxygen: It is obtained by difference.
Percentage of O = 100 - Percentage of (C + H + S + N + ash)
(3) Sulphur, although contributes to the heating value of coal, yet on
combustion produces acids (S02 and S03), which have harmful effects of
corroding the equipments and also cause atmospheric pollution. Sulphur is,
usually, present to the extent of 0.5 to 3.0% and derived from ores like iron
pyrites, gypsum, etc., mines along-with the coal.
Presence of sulphur is highly undesirable in coal to be, used for making
coke for iron industry, since it is transferred to the iron metal and badly
affects the quality and properties of steel. Moreover, oxides of sulphur
(formed as combustion products) pollute the atmosphere and leads to
corrosion.

(4) Oxygen content decreases the calorific value of coal. High oxygen-content
coals are characterized by high inherent moisture, low calorific value, and
low coking power. Moreover, oxygen is in combined form with hydrogen in
coal and thus, hydrogen available for combustion is lesser than actual one.
An increase in 1% oxygen content decreases the calorific value by about 1.
7% and hence, oxygen is undesirable. Thus, a good quality coal should have
low percentage of oxygen
 SIZE
Coke MICUM
Testing CRI COKE REACTIVITY INDEX

CSR COKE STRENGTH AFTER REACTION

COKE SIZE
The separation of coke pieces produced from the ovens for various
sizes is done by using screen.
Coke Porosity
The coke possesses pores of different sizes and nature. The porosity
affects the coke quality by providing surface area for reaction between
carbon and carbon dioxide gas. The pore volume and size affect the
strength of the coke.
The coke porosity is easily measurable by boiling water method. The
porosity test procedure is as follows:
A piece of solid dry sample is weighed in air (W 1 ). This solid material is
then- dipped in boiling water for 30 minutes. The boiling action will
cause expansion of air bubbles trapped in the pores and cause its
expulsion. Once the heating is stopped, the water cools and enters into
the pores to fill it completely. The weight (W 2 ) of the water saturated
sample is taken while dipped fully under water. The sample is now
taken out and surface water is removed by soaking with cotton cloth.
The weight of water saturated sample is taken in air (W 3 ).
Coke Strength
The coke strength is very important for its use in metallurgical furnaces.
The coke is handled, transported, stored and charged in furnace
mechanically. In all these operations, the coke particles breakdown to
smaller particles which is undesirable. The coke particles breakdown by
impact forces caused by dropping during handling coke and by shearing
force (wearing) during movement. The coke is tested for its ability to
sustain impact and wear actions by
(i) Shatter test(Impact strength) and
(ii) Tumbler test (Wear strength)
MICUM TEST
In this method, 50 kg coke sample (–75 to +50 mm size) is tested in
a drum (1000 mm diameter and 1000 mm wide) fitted with 4 lifters (100 mm
size). The drum is rotated at 25 rpm for 100 revolutions and the product is sized
by 60, 40, 20 and 10 mm screens and weighed. The strength values are
represented as:

The higher value of M 40 is indicative of good resistance to impact while higher

value of M 10 is indicative of poor resistance to abrasion. A coke with high M 40
and low M 10 value would be appreciated for use in blast furnace. The Micum 40
(M 40 ) index represents the tumbler index while the Micum 10 (M 10 ) index
indicates abrasion index.
COKE REACTIVITY INDEX(CRI)
Carbon reacts with oxidizing gases like carbon dioxide and steam to
yield gases like CO and H2 .
C + CO2 = 2CO
C + H2O = CO + H2
The coke reactivity is a measure of the rate at which coke carbon is able
to react to get converted into carbon monoxide gas. The coke reactivity
is important for its gasification to carbon monoxide to be used as
gaseous reducing agent in metallurgical furnaces. The coke reactivity
differs from coke combustibility.
CRI value should be about 20-25%
COKE STRENGTH AFTER REACTION(CSR)

The strength of coke is minimized due to reaction of cell wall carbon

with CO2 gas to generate CO gas. If this happens rapidly, then the cell
wall thinning may cause breaking of coke under load at high
temperature.

CSR Value should be above 60-65%

In the determination of CSR and CRI, 200 g of coke sample prepared as
per the standard size is reacted in a reaction vessel at 1100 °C in a CO2
atmosphere at a flow rate of 5 liters per minute (LPM) for 120 min. The
percentage weight loss after reaction is known as the coke reactivity
index (CRI). The reacted coke sample is then tumbled in an I drum for
600 revolutions at 20 RPM for 30 min and screened on a 10 mm round
screen. The % weight retained on the 10 mm screen is known as coke
strength after the reaction.

(M1-M2)*100 where M1 is the original test sample or weight

CRI = M1 before reaction; M2 is the sample mass or
weight after reaction in CO2; and M3 is the
sample mass or weight of +10 mm coke after
tumbling.