Bangladesh University of Engineering and Technology

Course No: CHE 402

Course Name: Chemical Engineering Laboratory-V
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Experiment No. 05

Name of the Experiment:

A. Calorific value of solid fuel by bomb calorimeter (ASTM D 2015-96)

B. Cloud point and pour point determination for diesel (ASTM D 2500-02)

C. Flash point and fire point for kerosene and diesel (ASTM D 93-02)

Date of Performance: 24.06.19

Date of Submission: 14.09.2019

Submitted To-

Dr. Md. Mominur Rahman

Professor

Department of Chemical Engineering, BUET

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 Name of the Experiment:

4D. Smoke point of kerosene (ASTM D 1322-97)

5A. Calorific value of solid fuel by bomb calorimeter (ASTM D 2015-96)

Partners’ Std. Id- 1502011 Prepared by,

1502012 Jannatul Osman Arju

1502013 Std, Id- 1502014

1502015 Level- 4, Term- 1

Dept. – ChE

Group 03 (A1)

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 4D. DESIGNATION: ASTM D 1322 – 97; STANDARD TEST METHOD
FOR SMOKE POINT OF KEROSENE

4. D.1 Objective

The aims of the experiment are to know about the quality of the sample and the ability of
kerosene sample to burn at complete combustion without smoking.

4. D.2. Scope

This test method covers a procedure for determination of the smoke point of kerosene and
aviation turbine fuel.

4. D.3. Terminology

Smoke Point

Smoke point is defined as the maximum flame height, in millimeters, of a smokeless flame of
fuel burned in a wick – fed lamp of a specified design.

Kerosene

Kerosene is petroleum distillate, boiling between 1400C and 300oC, generally used in lighting
and heating applications.

Aviation turbine fuel

Aviation turbine fuel is also refined petroleum distillate, generally used as a fuel for aviation
gas turbines

4. D.4. Significance

Smoke point is important from health hazard point of view or a longevity of an equipment.
For example, in boiler or furnace, fuels are burned for supplying heat. If the fuels produce a
lot of smoke, it will result in scale formation. As a result, the capacity and endurance of the
equipment will be affected. The smoke point test is a qualitative measure of a fuel
characteristics. So, one should have a clear concept about it.

This test method provides an indication of the relative smoke producing properties of
kerosene and aviation turbine fuel in diffusion flame. The smoke point is related to the
hydrocarbon type composition of such fuels. Generally, the more aromatic the fuel the

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smokier the flame. When the sample contains a big amount of aromatic compounds, it
produces a lot of smoke in a short time and the smoke point would be small and vice versa.
So a high smoke point indicates a fuel of low smoke producing tendency.

The smoke point is quantitatively related to the potential radiant heat transfer from the
combustion products of the fuel. Because radiant heat transfer exerts a strong influence on the
metal temperature of combustor liners and other hot section parts of gas turbines, the smoke
point provides a basis for correlation of fuel characteristics with the life of these components.

4. D.5. Apparatus

i. Smoke Point Lamp

It comprises a tripod stand, lamp body, and chimney. The measuring scale is viewed through
a curved glass window on the front of the instrument. A mirror can be attached to the
chimney to aid smoke detection. It is supplied with candle assembly and certified wick. The
top of the wick guide is exactly at level with the zero mark on the scale. The scale is marked
in white lines on black glass on each side of a white or black strip 2 mm in width. It has a
range of 50 mm graduated in 1 mm intervals, figured at each 10 mm and with longer lines at
each 5 mm.

ii. Wick

A woven solid circular cotton of ordinary quality, having the following characteristics:

Casing 17 ends, 66 tex by 3

Filling 9 ends, 100 tex by

Weft 40 tex by 2

Picks 6 per centimetre

iii. Pipettes or Burettes, Class A

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4. D.6 Experimental Set-up

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4. D.7. Procedure

An extracted and dried wick was soaked in the sample fuel. The sample was burnt in a
standard lamp in which the flame height could be varied against a background of a graduated
millimeter scale. The smoke was raised and smoke point was measured until a smoky flame
appeared and then to the point where the smoke just disappeared. The maximum flame height
was measured to the nearest millimeter considered as the smoke point of kerosene.

4. D.8. Observed data

Maximum flame height without smoke of kerosene = 23 mm

4. D.9. Result and Discussion

Result

In the experiment the smoke point of kerosene sample was found to be 23 mm

Discussion

The smoke point of kerosene found is very small. It gives the indication of lower quality of
the tested sample and tendency of incomplete combustion. The possibility of black soot
formation is higher for this sample. It also gives a qualitative measure of the high aromatic
and sulphur contents in the sample.

Some precautions should be taken while conducting the experiment to get reliable
experimental value and ensure safety. Such as, while placing the wick tube in the candle it
must be checked that the candle air vent is free from fuel since it may create fire. An efficient
device for lowering and raising the flame should be used to have smooth and regular
movement of the flame. To prevent the formation of multiple images, the glass window of the
door shall be curved. To eliminate errors due to parallax, the eye of the observer must be
slightly to one side of the center line, so that a reflected image of the flame can be seen on the
scale on one side of the central vertical white line, and the flame itself can be seen against the
other side of the scale. The joint between the base of the candle and the candle body needs to
be oil tight.

Recommendation
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A medium density cobalt glass may be used to reduce eye fatigue when observing the flame.
Automated scale can be used in lieu of manual measurement to have better accuracy.

5A.DESIGNATION: (ASTM D 2015-96); STANDARD TEST METHOD

FOR GROSS CALORIFIC VALUE OF SOLID FUEL BY THE
ADIABATIC BOMB CALORIMETER

5. A.1. Scope

1.1 This test method covers the determination of the gross calorific value of coal and coke by
the adiabatic bomb calorimeter
1.2 The values stated in SI units and British thermal units are to be regarded as the standard.
1.3 This standard does not purport to address the safety concerns of anyone associated with
its use. It is the responsibility of the user of this standard to establish appropriate safety and
health practices and determine the applicability and regulatory limitations prior to use
1.4 All accountability and quality control aspects of ASTM Guide D 4621 apply to this
standard

5. A.2. Terminology

Calorific Value: The heat produced by combustion of a unit quantity of a substance under
specified conditions. In the ASTM standard test method it is expressed in Btu/lb. units.
Calorific value may also be expressed in (cal/g) or in SI units (J/g) when required.

Gross calorific value: Gross heat of combustion at constant volume, Qv (gross). The heat
produced by combustion of unit quantity of a solid or liquid fuel when burned at constant
volume in an oxygen bomb calorimeter under specified conditions, with the resulting water
condensed to a liquid.

Net calorific value: Net heat of combustion at constant pressure, Q p (net). The heat produced
by combustion of unit quantity of a solid or liquid fuel when burned, at a constant pressure of
1 atm (0.1 MPa), under conditions such that all the water in the products remains in the form
of vapor.

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Corrected temperature rise: The temperature change of the calorimeter caused by the
process that occurs inside the bomb, i.e. the observed temperature change corrected for
various effects noted.

Energy Equivalent/heat capacity/water equivalent: The energy required to raise the

temperature of the calorimeter one arbitrary unit. This is the quantity that when multiplied by
the temperature rise, then adjusted for EΔT −e −e −e extraneous heat effects and
1 2 3
divided by the mass of the sample m gives the gross calorific value.

So, Gross Calorific value of Coal, Qv =

Where,

E = energy equivalent of the sample, cal/⁰C

ΔT= temperature rise in the calorimeter, ⁰C

e1 = Thermochemical energy corrections for the test for heat of formation of HNO3

e2 = Heat of formation of H2SO4 – heat of formation of HNO3

e3 = Heat of combustion of ignition wire

m = mass of sample (coal) taken, g

For calculation of the correct gross calorific value, proper allowances for heat contributed by
other processes and thermochemical corrections should be made. The thermochemical
corrections related to this experiment are discussed below shortly.

1. Energy of formation of Nitric Acid:

A correction e1 is applied for the acid titration. This correction is based on the assumptions:

a) That all the acid titrated is Nitric acid formed by the following reaction:

½ N2 (g) + 5/4 O2 (g) + 1/2 H2O (l) = HNO3 (in 500 mole H2O)

b) The energy of formation of HNO 3 in approximately 500 mole of water under bomb
conditions is -59.0 kJ/mole.

2. Energy of formation of Sulfuric acid:

By definition the gross calorific value is obtained when the product of the combustion of
sulfur in the sample is SO4 (in grams). However, in actual bomb combustion process, all the
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sulfur is found as H2SO4 in the bomb washings. A correction e3 is applied for the sulfur that is
converted to H2SO4 and this correction factor is calculated from the difference between the
heat of formation of H2SO4 from the heat of formation of HNO3 which is calculated to be 5.52
kJ/g of sulfur in the sample times weight of sample in grams times percent sulfur in sample.

The reaction takes place here is following:

SO2 (g) +1/2 O2 (g) + H2O (l) = H2SO4 + heat

The extent of this reaction and the amount of heat evolution depend upon the sulfur content
of the sample coal.

3. Fuse (ignition) wire:

The energy contribution for burning the fuse wire is calculated in accordance with the
directions furnished by the supplier of the wire. It is expressed by a correction factor e 3.
Generally for different wires the value of e 3 is calculated by multiplying the energy required
to burn the unit length of the specific wire with the length of the wire that has burned out.

5. A.3. Significance

i. The gross calorific value is used in computing the calorific value versus sulfur content to
determine if the coal meets regulatory requirements for industrial fuels.
ii. The gross calorific value is used to compute the total calorific content of the quantity of
coal represented by the sample for payment purposes, provided the buyer and the seller
mutually agree upon this.
iii. The gross calorific value can also be used for evaluating the effectiveness of beneficiation
processes or for research purposes.

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5. A.4. Apparatus

Combustion Bomb: It is constructed of materials that are not affected by the combustion
process or products sufficiently to introduce measurable heat input or alteration of end
products. The bomb is designed so that all liquid combustion products can be completely
recovered by washing the inner surfaces. There must be no gas leakage during the test. The
bomb is capable of withstanding a hydrostatic pressure test of 20 MPa at room temperature
without stressing any part beyond its elastic limit.

Calorimeter vessel: It is made of metal with a tarnish resistant coating, and with all outer
surface highly polished. Its size is such that the bomb becomes completely immersed in water
when the calorimeter is assembled. It has an electric device for stirring at a uniform rate but
minimum heat input.

Jacket: There is a double-walled, water filled jacket fully enclosing the calorimeter.

Thermometers: Thermometers are used to measure temperature in the calorimeter and

jacket.

Thermometer accessories: A magnifier is used for reading the thermometer to one tenth of
the smallest scale division.

Sample holder: It is an open crucible of platinum, quartz or acceptable base-metal alloy.

Ignition wire: Wire which is used to ignite the fuel.

Ignition circuit: Ignition circuit is used for ignition purpose provides 6 to 16 V alternating or
direct current to the ignition wire. A pilot light is required in the circuit to indicate the current
is moving.

Balance: A laboratory balance having capacity to weigh the sample to the nearest 0.0001 g.

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5. A.5. Experimental Setup

Figure 5.A.1: Schematic diagram of standard test method for gross calorific value of coal by
adiabatic bomb calorimeter

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5. A.6. Procedure

The bomb was rinsed, inverted to drain and left to dry. A measured length of ignition wire
was connected to the terminals, with enough slack to allow the ignition wire to maintain
contact with sample. The bomb was assembled and O 2 was charged at a pressure of 25 psi.
The calorimeter was filled with measured quantity of water (2000 g) adjusted from 1.0 to
2.0°C below from room temperature. The assembled bomb was placed in the calorimeter
vessel. It was checked that no O2 bubbles were leaking from the bomb. The calorimeter vessel
was then placed inside the water jacket. Then the electrodes were connected. The stirrer,
thermometer and cover of the vessel were placed in definite positions. The stirrer was started
then. The initial temperature reading just before igniting the wire was taken. When three
consecutive readings became same within one-tenth of smallest thermometer subdivisions
then it was assumed that the temperature had risen to its final equilibrium value and that
reading was taken. The cover was opened then, the bomb was removed and pressure was
released. The interior of the bomb was washed with distilled water containing titration
indicator. The combined pieces of unburned ignition wire were measured and subtracted from
the original length.

5. A.7. Observed Data

Mass of sample (coal), m = 1.0490 g

Initial temperature, Ti = 31.20oC

Final temperature, Tf = 34.00 oC

5. A.8.Calculated Data

Temperature difference = (Tf – Ti) ⁰C

= (34.00 – 31.20)⁰C

= 2.80 ⁰C

Calorific value = 6604.38 kcal/kg

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5. A.9. Sample Calculation

The energy equivalent of coal (the heat required to increase 1 oC temperature of 2000g water
by combustion), E = 2485 cal/ oC

Correction factors (added heat):

For heat of formation of HNO3, e1 = 10 cal (assume)

For (heat of formation of H2SO4 – heat of formation of HNO3), e2 = 10 cal (assume)

For heat of combustion of ignition wire = 2.3 cal/cm × (Li – Lf) cm = 10 cal (assume)

Temperature Rise, ΔT = (Tf –Ti) = (34.00 – 31.20) oC = 2.80 oC

EΔT −e1 −e 2 −e 3
Gross calorific value of sample coal, Qv = m

( 2485× 2.8 )−10−10−10

= cal/g
1.0490

= 6604.38 cal/g

= 6604.38 kcal/kg

5. A.10. Results and Discussions

The gross calorific value of the sample coal is found to be 6604.38 kcal/kg.

The amount of heat produced by different types of fuels on burning is expressed in terms of
calorific value. For a solid fuel, GCV (gross calorific value) is a very important characteristic
property because this value determines the grade of the fuel. The higher the calorific value,
the better the quality or grade of the fuel. Heat energy is evolved and transformed to many
other useful forms by burning a fuel through combustion reaction. So it is very significant in
selection of solid fuel when designing equipment or a plant & for finding out that whether it
can serve the purpose for that definite process. It also determines the economic and technical
applicability of the fuel for that particular process.

Among the different grades of coal, Anthracite is considered to be the best as it has the
highest heating value and carbon contents .Compared to the literature gross calorific value for
general Anthracite coal which is approximately 8600 kcal/kg, the calculated value for the
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given sample was 6604.38 kcal/kg. The deviation indicates that the sample coal varies in
composition from anthracite and has a higher degree of Sulphur content and unburned carbon
.The composition differs due to formation of coal from different source and in different
condition. Besides, for the calculation of the gross calorific value of the solid coal sample,
some correction factors for extra heat addition to the system by heat of formation of HNO 3
and also H2SO4, and also for the heat of combustion of the ignition wire were taken into
account. But the temperature correction factors for determining the actual temperature rise in
the calorimeter was not taken into account. It might be a reason of aberration in the calorific
value. It is important to keep the calorimeter vessel and the test bomb adiabatic fully, but it
was not possible in actual situation. As a result, a certain amount of heat loss could not be
prevented.

It is necessary to follow the ASTM standard testing method and maintain all the apparatus
handling and procedure steps very strictly to get better experimental result. Such as, the
supply rate of pressurized O2 gas in the bomb for combustion reaction should be uniform.
The gas has to be admitted into the bomb to prevent blowing of powdered material from the
sample holder. If the pressure exceeds the specified pressure, then the combustion reaction
should not be continued anymore.

During wire ignition , the wire must be in definite contact with the sample fuel, otherwise the
circuit will not be closed, and the pilot light will show that no current is passing through thus
no ignition is occurring.

Although, there were flaws in the experiment, but the method of determining calorific value
of solid fuel (coal) by ASTM method was done quite successfully.

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