Department of Chemical Engineering

Energy Laboratory
Subject Code: CHS651

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 CONTENT
Particulars Page No
Course Objectives & Outcomes 1
General Instructions to the Students 2
Syllabus 4
Guidelines for the preparation of laboratory reports 5
Experiment No: 1 Proximate analysis of coal 9
Experiment No: 2 Determination of shattering index of coke 12
Experiment No: 3 Study the caking index of coal 14
Experiment No: 4 Study the swelling index of coal 16
Experiment No: 5 Determination of the viscosity of the fuel oil 17
Experiment No: 6 Determination of flash point and fire point of an oil by 19
closed cup Pensky martin
Experiment No: 7 Determination of moisture content of fuel oil by dean 21
and stark apparatus
Experiment No: 8 Determination of aniline point of fuel oil 23
Experiment No: 9 Determination of vapor pressure of petroleum 25
products using REID apparatus
Experiment No: 10 Atmospheric distillation of petroleum product 28
Experiment No: 11 Determination of calorific value of solid fuel by bomb 30
calorimeter
Experiment No: 12 Determination of carbon residue of fuel by Conradson 32
method

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Course Objectives & Outcomes
I. Demonstrate and understand the principles of fuel properties testing instrument.
II. Conduct the experiments for determination of properties of different fuels.
III. Analyze the performance of equipment through group tasks.

CO

PO
a b c d e f g h i j k l m
I X X
II X X
III X X X

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 General Instructions to the Students
 Laboratory uniform, shoes & safety glasses are compulsory in the lab.
 Do not touch anything with which you are not completely familiar. Carelessness may not
only break the valuable equipment in the lab but may also cause serious injury to you and
others in the lab.
 Please follow instructions precisely as instructed by your supervisor. Do not start the
experiment unless your setup is verified & approved by your supervisor.
 Do not leave the experiments unattended while in progress.
 Do not crowd around the equipment’s & run inside the laboratory.
 During experiments material may fail and disperse, please wear safety glasses and
maintain a safe distance from the experiment.
 If any part of the equipment fails while being used, report it immediately to your
supervisor. Never try to fix the problem yourself because you could further damage the
equipment and harm yourself and others in the lab.
 Keep the work area clear of all materials except those needed for your work and cleanup
after your work.
 Before conducting any experiments, in the first lab students are instructed by the
laboratory technician and teaching assistants to abide by safety rules and take all necessary
precautions to ensure a safe work environment in order to safeguard their health, and the
health of their coworkers.
 This lab deals with boiling water hot surfaces, which can cause serious burns. All lab
instruments have been designed such that all exposed surfaces are well-insulated and not hot
to touch.

The safety precautions that the students are asked to follow include:
 Food, drinks, and related utensils are prohibited from being brought, stored or consumed
in the laboratory. Smoking is strictly prohibited in laboratories. Unauthorized individuals
must not be allowed in the laboratory. Laboratory must remain locked when unoccupied.
 Appropriate personal clothing, laboratory coats, gloves and personal protective
equipment (such as safety glasses) must be worn in the laboratory. Shoes must provide full
coverage of the feet. Laboratory coats must be removed and hands must be washed before
leaving the laboratory.

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 All occupants should be familiar with the locations and operation of safety and
emergency equipment such as fire extinguisher, first aid kits, emergency eye wash stations
and emergency showers, fire alarm pull stations, emergency telephone, and emergency exits.

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 National Institute of Technology Durgapur
Mahatma Gandhi Avenue, Durgapur - 713209, West Bengal.
Department of Chemical Engineering

ENERGY LABORATORY - SYLLABUS

Subject Code: CHS651 Exam Hours: 03
Hours/Week: 03 Viva Marks: 30
Total Hours: 30 Report preparation marks: 40
Experimental performance marks: 30

1. Proximate Analysis of Coal determines the moisture ash, volatile matter and fixed carbon
of coal in terms of weight percentage.
2. Shattering Index of Coke
3. Caking Index
4. Swelling Index
5. Viscosity of Fuel Oils
6. Determination of Flash point and Fire point of an oil by closed cup Pensky Martin
Apparatus
7. Determination of moisture content of fuel oil by Dean and Stark Apparatus
8. Aniline point determination by thin film
9. Determination of vapour pressure of petroleum products using Reid Apparatus.
10. To perform atmospheric distillation of petroleum product and to find out percent
recovery, percent total recovery, percent loss, percent residue.
11. Determination of calorific value of solid fuel by Bomb Calorimeter
12. Determination of carbon residue of fuel by Conradson Method

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 Guidelines for Preparation of Laboratory Reports
1. TITLE PAGE
The following items are to be included in the front page of the lab report according to this
order:
a) Student's name
b) Course and section Number
c) Number and title of the experiment
d) Date of the experiment
e) Names of group members
f) Date the report is presented
2. OBJECTIVE
The objective of the experiment should be stated on a separate sheet of paper with the
heading OBJECTIVE. State the objective clearly. A few explanatory sentences may be
included, if needed.
3. THEORY
In this section state and explain any equations or theoretical principles and assumptions that
were used in the experiment and the analysis. Define all parameters used.
4. EXPERIMENTAL PROCEDURE
Give a detailed description of how you accomplished the experimentation. This should
include equipment used in the experiment as well as how it was used. The description should
have sufficient details; so that another experimenter could duplicate your efforts. Use
sketches, diagrams, or photos to describe the experimental set-up. Label the main
components. Provide dimensions and material of test samples where applicable. The
equipment listing in the Appendices is the appropriate place for model numbers and serial
numbers. In the methods section, use generic names for the equipment, e.g., the fluid network
apparatus.
5. RESULTS
Summarize your results in an introductory sentence. Relate your results to your objective.
Present the results in the easiest way for your reader to understand: graphs, tables, figures,
etc. All tables and figures must be referenced in the text, use a numbering system for
identification of each one.
Explain the results of the experiment; comment on the shapes of the curves; compare results
with expected results; give probable reasons for discrepancies from the theory; answer any

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questions outlined in the instructions and solve any problems that may have been presented.
Tell why things happened, not only that they did happen. Comparisons should include
numerical values and corresponding error percentages where relevant.
Do not present calculations and formulas in this section. Your calculations should be detailed
in the Appendices under SAMPLE CALCULATIONS. Formulas should be discussed in the
THEORY section.
6. CONCLUSIONS
State your discoveries, judgments and opinions from the results of this experiment.
Summarize your primary results in comparison with theory in two or three sentences. These
should answer the objective of the experiment. Make recommendations for further study.
Suggest ways to improve the experiment.
Consider that in the real world, information like that in the RESULTS and CONCLUSIONS
will be all that upper management will want to receive. Beyond that, figures may be
skimmed. Make the most of these sections.

7. APPENDICES
A. DATA TABLES
Data tables are for the convenience of the extremely interested reader. These tables may
contain any additional comparisons or calculations that you have prepared and were not
included in the RESULTS section which may contain only summaries of your work. Data
Tables are the place to show everything that you did.
B. SAMPLE CALCULATIONS
Demonstrate how you performed the calculation made in the experiment. Include Show the
generic calculations to support all your work.
C. EQUIPMENT LIST
List every piece of equipment used in the experiment. Provide unique identification numbers,
when possible. State the accuracy and/or the readability of the instruments.
D. DATA SHEETS
Data sheets must be completed in ink and signed by the instructor at the completion of the
laboratory period. In the case of an error, line through the mistake, initial the mistake, and
continue. Record the name of the recorder and the group members on the raw data sheets.
8. PREPARATION OF GRAPHS
A. ORIENTATION
Plan the graph in so that the binding margin of the graph paper is at the left or at the top.
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B. COORDINATE AXES
Draw the axes of coordinates on the cross-sectioned part of the sheet, far enough in from the
margin to leave room for inserting the scales and their identifications between the edges of
the cross-sectioning and the axes, except when using log-log paper.
C. SCALES
Start all linear scales at (0,0) unless such a procedure would obscure the presentation of data.
Of course, this is not possible when using log scales. The units on the major divisions of log
scales should be powers of 10. Choose scales of 1, 2, 4, or 5 units per centimeter, or any
decimal multiples, such as 0.1, .002, and 400. Proper choice of scales is important. Guiding
principles are:
1. Utilize a good portion of the graph sheet area. DO not squeeze curves into one corner.
2. Do not unduly extend the scales. Have the scales readable to the precision of the
instruments from which data was taken. Further extension of the scales only scatters the data
points, emphasizing the experimental error.
3. Keep in mind the purpose of the graph. Avoid using scales that hide the real meaning or
fail to show the intended relationships.
4. Letter in the scale numerals along the axes, putting the abscissa scale beneath the
horizontal axis at appropriate intervals. Set all numerals on either axis in a vertical position as
viewed from the bottom of the page.
D. SCALE LEGEND
Letter in the abscissa legend beneath the abscissa scale so as to be read from the bottom of
the page. Letter in the ordinate legend to the left of the ordinate scale so as to be read from
the right hand of the page. If more than one ordinate scale is used, place each ordinate legend
immediately adjacent to the corresponding scale. Use descriptive titles followed by
dimensional units, e.g., CAPACITOR CURRENT (MILLIAMPS).
E. OTHER LETTERING
Use capitals for all lettering on the graph paper. Arrange all except scale legends to be read
from the bottom of the page and to run in horizontal lines.
F. TITLE
Letter in a concise descriptive title on each graph sheet, preferably in the bottom center. Do
not list the legends in the title.
G. DATA POINTS
Indicate data points by small circles or appropriate geometric symbols, except in the case of
correction curves for instruments where the plotted points are not emphasized.
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H. CURVES
Draw smooth curves whose positions are governed by the plotted points. The curves should
not necessarily pass through every point but should traverse the combined center of gravity of
all the points. Only in the case of perfectly smooth data will all the points lie on the curve.
One exception to the smooth curve rule: For instrument correction curves, join the plotted
points by straight-line sections and break the curve where it reaches the data points.
When more than one curve is drawn on the same set axes, carefully identify each curve,
preferable with a legend lettered immediately adjacent to the curve. Other (less desirable)
methods are to use horizontal legends, each with an arrow pointing to the appropriate curve,
or to number the curves and provide a table of titles. Data points for the different curves
should use different geometric symbols.
I. INDEPENDENT VERSUS DEPENDENT VARIABLES
Plot the independent variable horizontally along bottom of the graph. Plot the dependent
variable vertically. The dependent variable is usually mentioned first, e.g., "PRESSURE
VERSUS TEMPERATURE" where pressure is the ordinate.

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 EXPERIMENT NO: 1
PROXIMATE ANALYSIS OF COAL
OBJECTIVE:
To determines the moisture ash, volatile matter and fixed carbon of coal in terms of weight
percentage.
THEORY:
Proximate Analysis of a fuel determines the moisture ash, volatile matter and fixed carbon of
coal in terms of weight percentage. Based on these reports a number of information can be
determined on probable utilization of coal.
(a) Determination of Moisture:
Moisture means the water expelled from coal under specified condition without causing any
chemical reaction in coal. When a wet coal is exposed in atmosphere the external moisture
evaporates but the apparently dry coal still contains some moisture depends mainly on the
mode of occurrence and handling of coal, but the air dried moisture is related to the inherent
hygroscopic nature of coal.
Procedure:
Coal as available are crushed and sieved through -30 IS/ + 20 IS sieves. The mid portion is
then kept in the Laboratory racks in bottles with suitable labelling. This coal is used as
laboratory samples.
Apparatus:
An air oven in which a constant and uniform temperature of 105⁰C can be maintained for a
long time. One shallow glass dish with cover approximately 10 cm2 in area, and weight about
1gm, along with the lid.
Experiment:
A dry glass dish is taken and weighed. About 2gm of coal is weighed accurately by
difference. The coal is spread over the glass dish. The uncovered dish is heated in air oven at
105⁰C - 110⁰C for one hour. The dish is then covered while it is taken out from the air oven.
It is then cooled in a desiccator for 5-6 mins. And weighted when slightly warm.
(b) Determination of Ash Content:
Ash is the inorganic residue left when the fuel is heated in contact with air to a high
temperature under specified conditions. The bulk of the mineral matter of coal is due to clay
or shale consisting of aluminosilicates of different compositions. Other major constituents
may be calcite (calcium carbonate) and pyrites, or related matters. When coal burns, shale

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and other hydrated minerals lose water of hydration and sulphates, carbonates and sulphides
form oxides.
Apparatus:
Muffle Furnace:
Capable of giving a substantially uniform zone of 500 ⁰C in 30 minutes from the room
temperature and being raised in further 30-36 min. and maintained 815 ± 10 ⁰C in the next
30-60 mins. and maintained this temperature for 60 mins. The dish is then taken out cooled
and weighed.

(c) Determination of volatile matter:

Volatile matter does not include the moisture of coal but it contains water that is formed from
the hydrogen and oxygen of coal during the decomposition. The method consists of heating a
weighted quantity of air dried coal sample at a high temperature for a few minutes in absence
of air. When heated the organic and to some extent the inorganic substances of coal mass
dissociate and gaseous products are evolved. The loss in weight due to this evolution minus
moisture is stated as yield of volatile matter.

Apparatus:
(i) Muffle Furnace :
Capable of giving temperature of 900 ⁰C ± 15 ⁰C
(ii) Crucible :
Cylindrical silica crucible having height greater than diameter.
Procedure:
The crucible along with the lid is weighted and about one gram of coal is weighted accurately
by difference. Then with the lid, it is placed in the muffle furnace which is already heated to
900 ⁰C. The crucible with lid to be kept in the furnace at this temperature for 7mins. And then
the crucible is taken out, placed on a metallic plate for several minutes and then cooled in a
desiccator. This crucible is then weighted.
(d) Determination of Fixed Carbon :
Fixed carbon is the residue obtained by substracting from 100 the sum of percentages by
weight of moisture, volatile matter and ash. It is essentially carbon containing small amount
of nitrogen, sulphur, oxygen and hydrogen.
Fixed Carbon (F.C) = 100% - (M+A+V.M) %

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Observation:
W0 = Weight of glass dish with cover.
W1 = Weight of coal sample and glass dish.
W2 = Weight of dried coal sample and glass dish.
W3 = Weight of silica crucible with lid.
W4 = Weight of coal sample and crucible.
W5 = Weight of coal sample and crucible after heating.
W6 = Weight of silica dish.
W7 = Weight of coal sample and silica dish.
W8 = Weight of silica dish + Ash.

Calculations:
(i) % M. air dried =

(ii) A % air dried =

(iii) V.M. % air dried =

(iv) F.C. air dried = 100

(v) A% dry =

(vi) V.M. % dry =

(vii) F.C. % dry = 100

(viii) V.M. % d.a.f. =

(ix) V.M. % d.m.m.f. =

(x) F.C. d.a.f. = 100

(xi) F.C. d.m.m.f. = 100

Results: Report above results in tabular form

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 EXPERIMENT NO: 2
DETERMINATION OF SHATTERING INDEX OF COKE
OBJECTIVE:
To determine for one test sieve or for each of a number of test sieves of different sizes of
holes.
THEORY:
Shattering Index of Coke
As defined that coke has to be dropped from a specific height of 6’ (1.83) in a standard
equipment. The amount of coke should be 20 1b (9.0Kgs). The size of coke taken should be
above 2” (50 mm).The size distribution of the broken coke is determined and recorded.
This record gives the shattering index of the particular coke taken.
Apparatus:
We need shattering Index apparatus with standard dimension; weights for balancing the coke-
box. A balance and weights are required for weights of coke taken and different sizes of coke
taken. We need a set of sieves with aperture of 50mm, 40 mm, 25mm, and 12.5mm.
Procedure:
Lower of the coke-box and feed exactly 9.0 kg of above 50mm. size of coke whose shattering
Index to be determined. Next adjust the weights and raise the box so that the bottom of the
box is at a height of 1.83m from the big box at the bottom .Open the bottom door and allow
the coke to drop into the empty box at the ground. The broken coke are to be sieved with 50
mm, 40 mm, 25 mm, and 12.5 mm screens. This fraction are to be weighed and reported as
+50mm. -50mm.+40mm.-40mm. +25mm.-25mm.+12.5mm fractions. This give an idea of the
Shattering Index of the coke.
OBSERVATION
Size, mm. Feed Coke Shattered Code Remarks (if any)
Mass (gm.) Mass(gm)
Above 50mm.
-50mm. +40mm.
-40mm. +25mm.
-25mm. +12.5mm.
-12.5mm.
Total :

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RESULT:
(a) Now, calculate cumulative mass fraction (X) corresponding to 50mm., 40mm.,25mm,
and 12.5mm size. Plot X versus particle size and find cumulative mass fraction corresponding
to 37.5mm. from the plot (X37.5). Check whether X50 > 0.75, X37.5 > 0.85 and X12.5 > 0.97. If
so, it is a good quality B.F. coke.
(b) Find specific surface of feed coke (SF) and that of shattered coke(SP), taking density
of coke = 1.8gm/cc and sphericity = 0.73. Check whether (SP-SF) < 0.02 m2/kg. If so, it is a
good quality B.F. Coke.

NOTE: Specific surface =

= density, kg/m3
ᴪs= sphericity, dimension less,
xi = mass fraction of particles having average size, davg,i.

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 EXPERIMENT NO: 3
STUDY THE CAKING INDEX OF COAL
OBJECTIVE:
To determine the caking index of the coal.
THEORY:
The caking index of coal is identified as the maximum ratio of sand to coal which, after
carbonization gives a coherent mass capable of supporting a 500g weight and the proportion
of loose powder being less than 5% of the weight of sand and coal. It is understood that the
method provides only an approximate measure of the tendency of a coal to agglutinate. To
ensure reliable comparison it is necessary that comparative tests between different operations
should be carried out with the same batch of sand.
Apparatus: Silica crucible internal dia. at bottom = (26 +1) mm, height of crucible = (42 +
0.75) mm, silica triangle support; Muffle furnace, capable of maintaining a steady
temperature of 900° + 15°C; Rubber bung; 500g weight.
Sand: Should be of uniform quality, purity and shape.
Size: -30 + 20 I.S. sieve.
Procedure: The requisite quantities of sand and coal for a total amount of 15g, calculated
from the ratio given, is weighed and taken into a stoppered test tube. The ingredients are
mixed by the rotating the tube between the fingers and the thumb, until the mixture is of
uniform appearance. It is then poured into the silica crucible carefully, avoiding any
segregation. Finally careful mixing is done with the help of a spatula. The crucible is then
covered by the lid and put on the triangle and inserted into the furnace previously raised to
900° + 15°C. At the end of seven minutes, the crucible is withdrawn and cooled to room
temperature. After removing the lid a Rubber bung is placed with the narrower end resting on
the surface of the contents of the crucible. The crucible is then inverted on the Rubber bung
and the loose particles are allowed to fall on the glazed paper placed below. The solid cake
block is then lifted from the bung and placed over a porcelain tile and the weight 500g is
placed over it. If the cake residue is not broken, the weight of the loose material obtained on
the flared paper is then noted.
The test is repeated with different ratios of sand to coal for the total weight of 15g in each
case. The ratio which supports a weight of 500g with a proportion of loose material being less
than 5% of the weight of the mixture is reported as Caking Index; say 8 when the ratio is 8:1.

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Results:
Set Wt. of Wt. of Ratio Cake residue Wt. of % of Caking
No. coal (g) sand (g) sand : coal broken or not loose loose Index
material material

For example: Say ratio of sand : coal taken = 3:1

Wt. of sand = 11.25g
Wt. of coal = 3.75g

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 EXPERIMENT NO: 4
STUDY THE SWELLING INDEX OF COAL
OBJECTIVE:
To study the swelling index of the coal sample.
THEORY:
The swelling index number of coal is determined by this test. Swelling number test is
intended solely to give some comparative measure of the swelling properties of coals and is
based on the standardization carried out in United Kingdom in a number of laboratories using
wide variety of coals. This test is one of the indices for caking and swelling properties and
has been accepted by the Indian standard institution for Indian coals.
Apparatus:
Small silica crucible with lid.(capacity 15 ml. Approx).
Draught shield fitted with silica triangle.
Physical balance and weight box.
Procedure:
About 1gm. of coal is weighted roughly in the crucible and lightly tapped for 12 times on the
table to level the surface. The covered crucible is placed upright on the silica triangle
supported in the draught shield. The gas is lighted and heated for about 1 minutes with long
blue flame so that the flame reaches upto the lid of the crucible. The crucible is allowed to
cool and the coke button is then compared with standard profiles.

Swelling Index Profiles:

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 EXPERIMENT NO: 5
DETERMINATION OF THE VISCOSITY OF THE FUEL OIL
OBJECTIVE:
To determine the viscosity of the fuel oil.
THEORY:
Viscosity of Fuel Oil
When a fluid is flowing through a pipe or Channel, the successive layers of the fluid give
resistance to the flow which is manifested as viscosity (µ) of the fluid. The property has the
dimensions M/L/θ. In C.G.S. system the unit is gm/cm.sec, which is known as poise and in
F.P.S. system, it is (1b)/(ft) sec. As the unit of poise is very large in magnitude, the unit of
centipoise (C.P.) is used in practice. Relative viscosity is the ration of viscosity of the liquid
to that of water at 68 ◦F (20 ◦C). The viscosity of water at 20 ◦C (68 ◦F) is 1.002 C.P. When
the viscosity of fluid is divided by its density at the same temperature, it is termed as
kinematic viscosity (η) and its dimension becomes (M/Lθ)/(M/L3) = L /θ and unit is stokes.
The general practice is to use the term centi-stoke .
Apparatus: Redwood Viscometer:
The apparatus consists of metallic cup, having a small hole at the bottom. The hole can be
closed by a small ball –valve attached to a handle. The cup is provided with a level indicator.
For heating the liquid, water jacket with a stirrer is provided and the whole apparatus rests on
three levelling screws. Thermometers are provided to read the temperatures, 50 ml measuring
flask and stop watch are required.

Schematic Diagram of Redwood Viscometer Apparatus:

17
Procedure:
The oil cup is cleaned and thoroughly dried. Soft tissue paper or clean cotton should be used
for rubbing the interior of the cup .The apparatus is set up and levelled. The temperature is
adjusted to the required point , the stirrer in the bath being rotated continuously , and the oil
gently stirred by means of the thermometer while the temperature is being adjusted , but not
during the actual test . After the oil temperature hasbecome steady at the required value, the
level is accurately adjusted to the point of the gauge by allowing some oil to run out. A clean,
dry 50 ml flask is placed centrally below the hole, so that the neck is a few mm below the
bottom of hole. The valve is lifted and a stop watch is simultaneously started. As the oil
reaches the graduation mark on the neck of the flask,the watch is stopped, and a reading of
the oil thermometer is taken. The viscosity of an oil is to be expressed as the number of
seconds for the collection of 50 ml. When flowing under standard condition through a jet of
standard dimensions.
Take one reading at the room temperature and other at 20 ◦C. The kinematic viscosity of the
oil may be calculated from the formula:
( η ) = AØ – B/Ø, where η=kinematic viscosity of the oil in centistokes,
Ø = time of flow of 50 ml. in secs. And A and B are instrument constants.
For Ø= 40 to 85 secs, A = 0.264 and B = 190.
For Ø = 85 to 2000 secs, A = 0.247 and B = 65.
These constant are based on results worked out at a 21˚C, but it can be used for 20◦C - 60˚C
for engineering used safely.

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 EXPERIMENT NO: 6
DETERMINATION OF FLASH POINT AND FIRE POINT OF AN OIL
BY CLOSED CUP PENSKY MARTIN
OBJECTIVE:
To determine the flash point and fire point of an oil by closed cup Pensky Martin apparatus
(Closed cup flash point).
THEORY:
Flashpoint is the minimum temperature at which an oil or petro fuel gives out sufficient vapor
to form an inflammable mixture with air and catches fire momentarily i.e. flashes, when
flame is applied. Flash point of an oil gives an idea about the; nature of boiling point diagram
of the system, amount of low boiling fraction present in the liquid fluid, explosion hazards
during storage and handling, volatility of the liquid fuels. Fire point is the lowest temperature
at which vapors given of by oil ignites and continues to burn for at least 5 seconds. In most
cases, fire point is 5-40 ̊C higher than flash point and is determined in the same apparatus as
for flash point determination. It gives an idea of fire hazards during the storage and use of oil.
Pensky martin apparatus is used for determination of flash point above 50 ̊C.

Apparatus: PENSKY MARTIN Apparatus

Accessories/Chemicals Required: Thermometer-1 no, Gas lighter, Lube Oil.
Procedure:
1. Thoroughly clean and dry all parts of the cup and its accessories before starting the test.
2. Fill the cup with sample to be tested to the level indicated by the filling mark.
3. Place the lid on the cup and set the latter in the above.

19
4. Insert the thermometer. Light the test flame and adjust it to 4mm in diameter.
5. Supply the heat by energy regulator at such a rate that the temperature as indicated by the
thermometer increases 5-6 ̊C per min.
6. Turn the stirrer stirring by means of hand in downward direction.
7. Apply the test flame by operating the mechanism on the cover which controls the shutter
and test flame burner so that the flame is lowered into the vapor space of the cup.
8. Do not stir the sample while applying the test flame. Record the flash point temperature
read on the thermometer at the time of test flame applicati0n causes a distinct flash in the
interior of the cup.
9. Continue the heating until the oil ignites and continues to burn for 5 seconds. Record the
temperature of the oil when this occurs, as the fire point.

Observation:
Serial No. Temperature Inference

CONCLUSION:

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 EXPERIMENT NO: 7
DETERMINATION OF MOISTURE CONTENT OF FUEL OIL BY
DEAN AND STARK APPARATUS
OBJECTIVE:
To determine of moisture content of a fuel oil by Dean and Stark Apparatus
THEORY:
Water solubility in oil is very low. However, it is present in fuel oil up to 1% in disperse
state. Undesirable oil is separated from oil by preheating. Dean and Stark method is used for
its determination in which oil sample is heated with carrier liquid which forms an azeotrop
with water. The distilled vapor on condensation and settling gives water as a separate layer
which is measured.
The presence of water in fuel oil is undesirable because, among other harmful effects arrival
of water globules at the outlet of an oil burner may lead to flame failure (the flame is
extinguished). The amount of water present in oil is determined by dissolving the oil in
carrier liquid and distilling all the water and some carrier liquid.
In common form of apparatus the distillation flask is fitted with a vertical, but offset, the
reflux condenser which discharge into vertical, graduated tube. Water collects at the bottom
of the tube and is measured, while excess carrier liquid is returned to the boiling flask.
This method is especially applicable to the crude petroleum’s and product derived from them
such fuel oil, road oil, road tar, asphalt and tars.

Schematic Diagram of Dean-Stark Apparatus

Apparatus: Dean and stark Apparatus.

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Accessories/Chemicals Required: Carrier liquid, fuel oil, Connection for cold water, Energy
regulator
PROCEDURE:
1. Measure 100ml of sample into distillation flask; rinse the measuring cylinder with 100ml
of carrier liquid in successive portions and add the washings, add a little broken pumic or
other suitable material.
2. Insert a loose plug of cotton wool in the top of the condenser tube to prevent the
condensation of the atmospheric moisture in the condenser tube.
3. The condenser tube and trap must be chemically clean to ensure free drainage of water
into the bottom of the trap.
4. Make all connections vapor and liquid tight after the components of the apparatus are
assembled.
5. Circulate cold water through the jacket of the condenser.
6. Heat the flask and regulate the heating so that the condensate falls from the end of the
condenser at the rate of 2 to 5 drops per second. Continue heating the sample until the volume
of the water in the receiver remains constant for 5 minutes. Wash down with the carrier liquid
any water adhering to the condenser tube.
7. When the volume of the water remains constant, remove the source of heat from the flask
and allow the receiver contents to cool to room temperature.

Carrier Liquid:
2T Oil/ super TT oil
Calculation and Reporting:
The volume of water in the trap is read to the nearest scale division and the water in the
sample is reported as percent by volume.
%of water= (volume of water in trap/volume of sample)*100
Report the result as a % by volume for the test liquid , that is, as the water content, IP
74, stating the amount of sample used in the determination.

Precaution:
As the carrier liquid and the fuel oil are highly inflammable, these materials are to be handled
with proper care. No ignition flame is allowed near the apparatus.

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 EXPERIMENT: 8
DETERMINATION OF ANILINE POINT OF FUEL OIL
OBJECTIVE:
To determine the aniline point by thin film.
THEORY:
The aniline point of an oil is the lowest temperature at which at oil is completely miscible
with an equal volume of aniline. It is the measure of the aromatic content of the oil, hence is a
characteristics property of diesel. The higher aniline point indicates lower aromatic content
and higher paraffin content. The higher is the aniline the better is the diesel fuel and the
lubricant. Aniline point of an oil gives an indication of the possible deterioration of rubber
sealing, packing etc. ion contact with the oil.
Apparatus/Chemicals required: Thermometer-Aniline point tube, thermometer, aniline,
Diesel, measuring devices.

Schematic Diagram of Aniline Point Apparatus

Procedure:
1. Dry the apparatus thoroughly in an oven at 150 °C and change it with the 5mlm of dried
sample and 5ml of aniline.
2. Close the tube by means of the bung and fit the thermometer.
3. Allow the mixture to warm by energy regulator at rate note exceeding 1 °C per min,
stirring constantly until the thermometer bulb can be seen by reflected light. Note this
temperature as aniline point.

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4. Cool the solution with stirring condition until the mixture becomes opaque. Note the
temperature as aniline point.
Take the average of these two temperatures, which gives the correct aniline point.
Observation:
Serial no. Temperature Inference

Precautions:
1. Aniline is extremely toxic and must be sucked.
2. Avoid overheating of solution.

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 EXPERIMENT NO: 9
DETERMINATION OF VAPOUR PRESSURE OF PETROLEUM
PRODUCTS USING REID APPARATUS
OBJECTIVE:
To determine the vapor pressure of volatile, non-viscous petroleum products.
THEORY:
Reid apparatus is used to determine the vapor pressure of volatile, non-viscous petroleum
products except liquefied petroleum gases, for which it gives low results. The sample is
contained in the gasoline chamber of the apparatus. The gasoline chamber is connected to an
air chamber fitted with a pressure gauge. Fixed temperature is maintained by hating the water
bath through which heat transfer occurs conventionally to the gasoline chamber. A stirrer is
used to transfer the heat uniformly throughout the water bath. After certain time a constant
reading is obtained on the pressure gauge.
In the measurement of the Reid Vapor Pressure (said to be absolute vapor pressure) there is
contrary to the true vapor pressure of the product---- an error due to fact that the Reid method
only vaporizes the light fractions at a measurement temperature 37.8C. The fractions of
components which is impossible to vaporize remains in the measuring chamber (non-volatile
fractions), with a vapor pressure which is lower than the product sample. The ratio of ‘true’ to
Reid vapor pressure is thus dependent on the sample composition.
Air chamber:
The upper section of the vapor pressure bomb. It is a cylinder vessel of approx.52mm internal
diameter and approx.254mm length. The one end of the cylinder is tapped with a 6mm
standard pipe-thread to receive gauge coupling. The other has an opening approximately
13mm diameter, and provided with means of coupling with the gasoline chamber. The air
chamber must drain completely from either end when held in a vertical position and for this
reason the inner surfaces of the must be slightly sloped to provide complete drainage when
inverted.
Gasoline-chamber:
It is the lower section of the vapor-pressure bomb. It has the same diameter as the upper
chamber and approx.64mm in length. The chamber has an opening approx. 13mm diameter at
one end, which is provided with the means of coupling with the air chamber. The inner
surface of the end containing the coupling member shall be sloped to provide complete
drainage when inverted.

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Pressure Gauge:
A bourdon type pressure gauge of test gauge quality approx. 102-152mm diameter, with a
passage-way not less than 4.5mm diameter from the Bourdon tube to the atmosphere. The
range of gauge to be used depends upon the vapour pressure of the sample.
Apparatus:
Air chamber, Gasoline chamber, pressure gauge, cooling bath, water bath, temperature
measuring instrument, stirrer etc.
Accessories/chemicals required: volatile, non-viscous petroleum products (such as petrol,
diesel etc.), ice, distilled water etc.
PROCEDURE:
1. Before placing new apparatus in service test the assembled vapor pressure bomb for
freedom from leaks by filling with air to 100 psig and immersing it in water bath. Use the
apparatus only if it stands up to this test without any leakage.
2. Rinse the air chamber with clean water which is preferably, at room temperature, unless
the sample to be tested is known to contain alcohol or other water soluble constituents. For
this rinse both the air chamber and the gasoline chamber with alcohol and then acetone are
and dry them by blowing air through them. Attach the bourdon type pressure gauge ensuring
that the connection is air tight.
3. Pour the water-bath with water up to the mark and start heating.
4. Set the temperature of the water bath by digital temperature controller and stir it with the
help of the stirrer attached with the apparatus.
5. Remove the gasoline chamber with air chamber and pour it with oil sample whose vapor
pressure is to be measured.
6. Connect the gasoline chamber with air chamber and cool the gasoline chamber by
placing it on an ice-water bath.
7. After reaching the desired set point (37.8 °C) place the assembled vapor pressure
apparatus inside the water-bath (keeping the gasoline chamber immersed in the water bath)
for 5 min.
8. Tap the gauge lightly and observe the reading.
9. Withdraw the bomb from the bath, invert it and shake it vigorously for 5 sec and replace
it in the bath in the shortest possible time to avoid cooling the apparatus.
10. Then at intervals of 2 min repeat this gauge observation and agitation and continue until
consecutive readings are same and equilibrium has been reached.
11. Record the gauge reading at equilibrium as the uncorrected vapor pressure in pounds.
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CALCULATION AND REPORTING:
In case of Bourdon pressure gauge; correct the value of the uncorrected vapor pressure by
adding the gauge correction.

Correction factor =

Where t is the initial air temperature

T = Temperature at which determination is made, °C
Pt = Vapor Pressure of water in psia at t °C.
PT = Vapor Pressure of water in psia at T °C.
Pa = Barometric Pressure in psia.

PRECAUTIONS:
1. Handle all the petroleum products carefully since these are highly inflammable.
2. Proper care should be taken while dismantling and assembling the bomb. Try to
complete this operation as early as possible.
3. Cool the sample properly before placing it inside the bath.
4. While withdrawing the bomb from the bath; make sure that the stirrer is switched off.
Removing the bomb at the time of the rotation of the stirrer may damage the blades of the
stirrer.
5. Make sure that the gasoline chamber is immersed in the water bath.

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 EXPERIMENT NO: 10
ATMOSPHERIC DISTILLATION OF PETROLEUM PRODUCT
OBJECTIVE:
To perform atmospheric distillation of petroleum product and to find out percent recovery,
percent total recovery, percent loss, percent residue.
THEORY:
In the distillation test a measured volume of the oil is distilled at the specified rate which is
suitably increased as the distillation proceeds. The initial boiling point (I.B.P) is the
temperature when the first drop of condensed liquid drops from the condenser and the final
boiling point (F.B.P) is the maximum temperature recorded at the end of distillation. Mid
boiling point is the temperature at which 50% of the oil distils off.
Distillation data are used for, making important curves like true boiling point curve,
equilibrium/flash vaporization curve. T.B.P. curve gives the variation of boiling point with
the yield of distillates. Each point in the flash vaporization curves, gives the total amount of
vapour in the equilibrium with the liquid at the particular temperature. These curves are used
in the design of continuous distillation equipments in Refineries.
Distillation characteristic is a measure of volatility of petro fuels and indicates the vapour
losses during fuel storage and vapour locking tendency.

APPARATUS: Atmospheric Distillation Apparatus

ACCESSORIES/CHEMICALS REQUIRED: Distillation flask, condenser and cooling
bath, energy regulator, graduated cylinder, thermometer.
PROCEDURE:
1) A 100 ml sample is measured in a graduated cylinder and to be poured into the
distillation flask.
2) Condenser and the thermometer are to be fitted with the distillation flask.
3) Apply heat to the distillation flask and contents by means of energy regulator. The
heating at this stage must be so regulated that the time interval between the first application
of heat and the initial boiling point does not exceed 5-10 min.
4) Continue to regulate the heating so that the time required from initial boiling point to 5%
recovered is 60-75 sec.
5) Continue heating at a rate so that time required for uniform average rate of condensation
from 5% recovered to 5 ml residue in flask is 4-5 min.

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6) When the residual liquid in the flask is approximately 5ml, make a final adjustment of
heat, if necessary, so that the time required from the 5ml of residue in the flask to the end
(final boiling) point shall be 3-5 min.
7) Observe and record the final boiling point or dry point or both, as required, and
discontinue the heating.
8) While the condenser tube continues to drain into the graduated cylinder, observe the
volume of condensate at 2 min interval until two successive observations agree.
9) Measure this volume accurately which represents present recovery. Deduct the percent
recovery from 100 to get “percent residue and loss”.
10) After the flask has cooled pour its contents into the condensate in the graduated cylinder
and allow draining until no appreciable increase in the volume of liquid in the graduated
cylinder is observed. Record this volume as percent total recovery. Deduct the percent total
recovery from 100 to obtain the percent loss.
11) Note and record the barometric pressure during the experiment in mm of Hg.

REPORTING:
Report from experimental result 1. Percent recovery. 2. Percent residue and loss. 3. Percent
total recovery. 4. Percent loss, 5.I.B.P.,F.B.P., temp at which 50% distillate recovered.

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 EXPERIMENT NO: 11
DETERMINATION OF CALORIFIC VALUE OF SOLID FUEL BY
BOMB CALORIMETER
OBJECTIVE:
To determine the calorific value of solid fuel by bomb calorimeter
THEORY:
A bomb calorimeter will measure the amount of heat generated when matter is burnt in sealed
chamber (Bomb) in an atmosphere of pure oxygen gas.

Schematic diagram of Bomb Calorimeter Apparatus

Apparatus:
a) Calorimeter Bomb b) Calorimeter vessel
c) Water jacket with cover and motorized stirrer.
d) Fuel cup. (Crucible) e) Oxygen filling device with copper filling.
f) Ignition system (firing unit) g) Digital thermometer.
h) Bomb lifting hook i) Briquate press.
j) Bomb lifting hook k) Ignition wire.
l) Firing Cotton.

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Procedure:
a) Fill the water jacket with distilled water up to the over flow mark.
b) Weight the fuel cup (empty crucible)
c) Weight the sample +fuel cup.
d) With help of pipette pour 1ml-distilled water in to the bomb .Place the fuel cup in the
circular ring support attached to the terminals of bomb. Attach a length of ignition wire
across the terminal under light tension .Take a suitable length of dry firing cotton and tie it at
the center of ignition wire. Touch the free end of the firing cotton to the sample in the fuel
cup pour a small quantity of water in to the bomb gasket and immediately close the bomb
securely.
e) Admit oxygen slowly with the help of oxygen filling devise to gauge pressure 30kg/cm2.
f) Fill the calorimeter vessel with standard quantity of distilled water as derived from
National Test House.
g) Place the prepared bomb in calorimeter. vessel with the help of bomb-lifting hook and
make the appropriate electrical connection to bomb electrode and firing unit .Put the cover in
position and arrange the digital thermometer sensor and stirrer so they do not touch bomb and
vessel.
h) Connect the three -pin top of firing unit to AC 220 volt. Put on the main switch and red
LED inductor will glow and simultaneously green LED will also glow and volt show the
voltage. Put on the stirrer switch and stirrer will start running. Digital thermometer will show
the temperature.
i) The temperature will increase slowly. When the temperature becomes steady the unit is
ready to firing. Note the steady temperature before firing(T1)
j) Press the firing switch (Fire Push). The green LED will go off and the voltmeter will show
“0”reading the temperature will start rising first at a quick pace and then slowly. Record the
temperature at 1 minute interval and note the highest temperature (T2).

Calculation:
Calorific value of sample

Where, w= water equivalent of calorimeter which is mentioned in N.T.H Certificate = 6256

joule/kelvin
T1= Initial temperature before firing.
T2= Highest temperature after firing

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 EXPERIMENT NO: 12
DETERMINATION OF CARBON RESIDUE OF FUEL BY
CONRADSON METHOD
OBJECTIVE:
To determination of carbon residue by Conradson method.
Theory:
It is the percentage of carbonaceous residue formed after evaporation and pyrolysis of a
petroleum product. This determination is important for fuel moil, lubricants, cracking feed
stock etc. Carbon deposits fouls the surface, results in wear and choking of cylinder and
affects the regeneration of cracking catalysts as it gives an indication of relative coke forming
tendency on evaporation and pyrolysis of oil. It is also a measure of carbon depositing
tendency of fuel oil and engine deposits fuel fired engine. It is determined by Conradson
apparatus and Rams Bottom Apparatus.

Schematic Diagram of Conradson apparatus:

Apparatus: Conradson apparatus

Accessories/chemicals required: Thermometer, burnt lube oil, tongues, hand gloves,
weighting balance, desiccators.

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Procedure:
1. Weigh 5gm-10gm sample of oil to be tested, free of moisture and other suspended
matter.
2. Place the crucible into a porcelain crucible containing two glass bids about 0.1Inch in
diameter.
3. Place this crucible in the center of skid more crucible.
4. Level the sand in the large sheet iron crucible and se t the skid more crucible on it in the
exact center of iron crucible.
5. Apply covers to both the skid more and the iron crucible, the one on the later fittings
loosely to allow free exit to vapors as formed.
6. On a suitable place the nichrome wire triangle.
7. Place the crucible setup on the nichrome wire triangle.
8. Cover the whole with iron hood in order to distinguish the heat uniformly during the
process.
9. Apply heat with a high, strong flame from themeker type gas burner, so that the pre
ignition periods will be 10+/-1.5min. When smoke appears above the chimney, immediately
move or tilt burner. Heat may be increased, if necessary when the flame does not show above
the chimney. The period of burning the vapors shall be 13+/-1.0 min.
10. When the vapor cease to burn and no further blue smoke can observed, readjust the
burner and hold the heat as at the beginning so as to make the bottom and lower part of the
sheet iron crucible a cherry red, and maintain for exactly 7 minutes. The total period of
heating shall be +/-2.
11. Remove the burner and allow the apparatus to cool until no smoke appears, and the
remove the cover of the skid more crucible (15mins).
12. Remove the porcelain crucible with tongue, place in the desiccators, cool and weight.
13. Calculate the percentage of carbon residue on the original sample.
Calculation and Report:-
Ax100
Carbon residue=…………………………………………… W
Where, A=weight of carbon residue obtained in gms
W=Weight of sample in gms
Report the value obtained as “Conradson Carbon Residue”

33