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Shahjalal University Of Science & Technology


Sylhet-3114
Dept. of Chemical Engineering & Polymer Science

Course Title: Fuel and Energy Sessional


Course No. : CEP 325

Lab Report
Dr. Engr. Salma Akhter

Submitted To:
Mithun Chandra Bhoumick

Professor
Dept. of CEP

Lecturer
Dept. of CEP

Submitted By:
Reg no. :
2012332001
2012332007
2012332008
2012332054
2012332055
2012332057
2012332062

Group-07
Name:
Sayeed Ahmed Sourove
Md. Abdus Samad Azad
Ahsan Habib
Md. Zarifuzzaman
Musabbir Jahan Talukdar
Md. Loshanur Rahman
Sudipta Mitra

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INDEX
No.

Name of the Experiment

Page No.

1.

Determination of moisture content, volatile


matter content, fixed carbon content of coal.

07-15

2.

Determination of aniline point.

16-18

3.

Determination of cloud point and pour point


of palm and soya bean oil.

19-22

4.

Determination of flash point and fire point of


kerosene.

23-25

5.

Determination of kinematic viscosity of


some oil.

26-30

6.

Determination of calorific value of ethanol


using bomb calorimeter.

31-35

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Safety

Safety:
Safety is the state of being safe ,the condition of being protected against physical,
social, spiritual, financial, political, emotional, occupational, psychological,
educational or other types or consequences of failure, damage, error, accident ,harm or
any other event which could be considered non-desirable. Safety can also be defined
to be the control of recognized hazards to achieve an acceptable level of risk. But in
laboratorial fact it defines slightly different thing. For laboratorial fact, safety means,
Isolates users from heat, sharp edges, hazardous energy (such as uv, microwave, etc)
and hazardous materials.
MSDS (Material Safety Data Sheet):
A material safety data sheet (MSDS) is an important component
of product stewardship and occupational safety and health. It provides guidance for
handling a hazardous substance and information on its composition and its properties.
It intended to provide workers and emergency personal with procedure for handling
or working with that substance in a safe manner and includes information such as
physical data (melting point, boiling point, flash point, etc), toxicity, and protective
equipment procedure. The MSDS follows a 16 section format which is internationally
agreed and for substances especially, the MSDS should be followed with an Annex
which contains the exposure scenarios of this particular substance.
The 16 sections are:

SECTION 1: Identification of the substance/mixture


1.1. Product identifier
1.2. Relevant identified uses of the substance or mixture and uses advised
against
1.3. Details of the supplier of the safety data sheet
1.4. Emergency telephone number
SECTION 2: Hazards identification
2.1. Classification of the substance or mixture

2.2. Label elements


2.3. Other hazards
SECTION 3: Composition/information on ingredients
3.1. Substances
3.2. Mixtures
SECTION 4: First aid measures
4.1. Description of first aid measures
4.2. Most important symptoms and effects, both acute and delayed
4.3. Indication of any immediate medical attention and special treatment
needed
SECTION 5: Firefighting measures

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5.1. Extinguishing media


5.2. Special hazards arising from the substance or mixture

5.3. Advice for firefighters

SECTION 6: Accidental release measures


6.1. Personal precautions, protective equipment and emergency procedures
6.2. Environmental precautions
6.3. Methods and material for containment and cleaning up
6.4. Reference to other sections

SECTION 7: Handling and storage


7.1. Precautions for safe handling
7.2. Conditions for safe storage, including any incompatibilities
7.3. Specific end use(s)

SECTION 8: Exposure controls/personal protection


8.1. Control parameters
8.2. Exposure controls

SECTION 9: Physical and chemical properties


9.1. Information on basic physical and chemical properties
9.2. Other information

SECTION 10: Stability and reactivity


10.1. Reactivity
10.2. Chemical stability

10.3. Possibility of hazardous reactions


10.4. Conditions to avoid
10.5. Incompatible materials
10.6. Hazardous decomposition products

SECTION 11: Toxicological information


11.1. Information on toxicological effects

SECTION 12: Ecological information


12.1. Toxicity
12.2. Persistence and degradability

12.3. Bioaccumulative potential


12.4. Mobility in soil
12.5. Results of PBT and vPvB assessment
12.6. Other adverse effects

SECTION 13: Disposal considerations


13.1. Waste treatment methods

SECTION 14: Transport information


14.1. UN number
14.2. UN proper shipping name
14.3. Transport hazard class(es)

14.4. Packing group

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14.5. Environmental hazards


14.6. Special precautions for user

SECTION 15: Regulatory information


15.1. Safety, health and environmental regulations/legislation specific for the
substance or mixture
15.2. Chemical safety assessment

SECTION 16: Other information

General safety procedure for the laboratory:

Safe work practices


Keeping the laboratory clean
Organized and functioning properly can help to prevent incidents and
injuries
. Never work alone in the laboratory
Unattended experiment
Only do the experiment which is desired.
Never do any experiment without knowing about the component.
Read all procedures carefully before doing the experiment.
Safe use and disposal of sharps
Never handle broken glass with your bare hands
Examine glassware before each use.

Never use chipped, cracked, or dirty glassware.

Do not immerse hot glassware in cold water


Safe use of laboratory equipment

All chemicals in the laboratory are to be considered


dangerous. Avoid handling chemicals with fingers. Always use a
tweezer.

Never remove chemicals or other materials from the laboratory area.


Never return unused chemicals to their original container.
Check the label on all chemical bottles twice before removing any of
the contents.

Electrical safety
Careful before operating any high voltage equipment.
Maintain an unobstructed access to all electrical panels.
Never modify, attach, or change any high voltage equipment.
Always make sure all capacitors are discharged before touching high
voltage equipment.
Avoid using extension cord whenever possible.
Chemical safety
Treat every chemical as they are hazardous.

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Never smell a solvent.


Never allow a solvent come to a contact with your skin.
Personal protective equipment:
Gloves.
Eye safety goggles.
Skin protection.
Foot protection.

Safety is an important term for our laboratorial work. We must work in


lab very safely thus no accident can happen. For these reason we need to learn safety
method very carefully. So, working safe and sound we should be aware those terms
of safety very carefully.

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Experiment no.-01
Determination of Moisture content, Ash content, and Volatile matter content of
coal.

Abstract
The moisture content, ash content and volatile matter content of a coal was determined
by following ASTM standard method in our experiment. For this we measured the
amount of coal in a crucible given by lab assistant after properly weighing the crucible.
As the weight of coal was needed after the coal being treated with different
temperature, we measured the weight of coal four times. Every time the weight was
subtracted from the previous one to determine the moisture content, carbonaceous
matter, ash content and volatile matter content. For treating coal with different
temperature we used dryer and muffle furnace. Finally the values of the moisture
content, carbonaceous matter, ash content and volatile matter content were calculated
in percentage.

1. Introduction:
A fuel is any material that can be made to react with other substances so that it
releases chemical or nuclear energy as heat or to be used for work. The concept was
originally applied solely to those materials capable of releasing chemical energy but
has since also been applied to other sources of heat energy such as nuclear
energy (via nuclear fission or nuclear fusion).The heat energy released by reactions
of fuels is converted into mechanical energy via a heat engine. Other times the heat
itself is valued for warmth, cooking, or industrial processes, as well as the
illumination that comes with combustion. Fuels are also used in the cells of
organisms in a process known as cellular respiration, where organic molecules are
oxidized to release usable energy.
Coal is a combustible black or brownish-black sedimentary rock with a high amount
of carbon and hydrocarbons. Coal is classified as a nonrenewable energy source
because it takes millions of years to form. Coal contains the energy stored by plants
that lived hundreds of millions of years ago in swampy forests. The plants were
covered by layers of dirt and rock over millions of years. The resulting pressure and
heat turned the plants into a substance now known as coal.[1] There are several
different types of coal that have different properties usually dependent on their age
and the depth to which they have been buried under other rocks. In some parts of the
world (for example New Zealand), coal development is accelerated by volcanic heat
or crustal stresses. The degree of coal development is referred to as a coals rank,
with peat being the lowest rank coal and anthracite the highest.[2]

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Figure: Formation of coal

2. Theory:
Coal varies widely in its composition. It is composed chiefly of rings of six carbon
atoms joined together in an extremely complex composition of layered arrangements
that have in them, not only hydrogen but significant amounts of oxygen and
nitrogen. The structure also includes varying amounts of sulphur and other
environmental pollutants. Up to one tenth of the total mass of coal can be material
with no fuel value. Coal is usually analyzed for moisture, volatile matter, fixed
carbon and ash. . The most basic analysis carried out to determine characteristics of
a coal is called proximate analysis.[3]
2.1. Moisture content:
Moisture is an important property of coal, as all coals are mined wet.
Groundwater and other extraneous moisture that coal absorbs are known
as adventitious moisture and are readily evaporated when coal is heated
to 100-120oC. The adventitious moisture can be held in coal body in the
form of:
Surface moisture: water held on the surface of coal particles
Hydroscopic moisture: water held by capillary action within the micro
fractures of the coal
Moisture held in chemically bonded form inside the coal is known as
inherent moisture. Inherent moisture is not removed at low temperatures
(100-1200C), it gets released at higher temperature during the combustion
of coal. It can be in the form of:
Decomposition moisture: water held within the coal's decomposed
organic compounds
Mineral moisture: water which comprises part of the crystal structure
of hydrous silicates such as clays Total moisture is analyzed by loss of
mass when coal is heated.[1]
The moisture content of coal ranges from 6% by
weight in anthracite coals to 45% by weight in lignite.
There are various standardized tests to determine the moisture content of
coal and they are classified depending upon the type of moisture
content tested
(1) ASTM D-1412 (ISO 1018) for determination of the
equilibrium moisture of coal at 96 to 97% relative humidity and
30C,

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(2) ASTM D-1412 (ISO 1018) for determination of the


equilibrium moisture of coal at 96 to 97% relative humidity and
30C,
(3) A S T M D - 3 1 7 3 f o r determination of the moisture in the analysis
sample of coal and coke,
(4) ASTM D-2961 for determination of the total moisture o f c o a l [ 4 ]
2.2. Ash content:
Ash content of coal is the non-combustible residue left after coal is burnt.
It represents the bulk mineral matter after carbon, oxygen, sulfur and
water (including from clays) has been driven off during combustion.
Analysis is fairly straight forward, with the coal thoroughly burnt and the
ash material expressed as a percentage of the original weight. It can also
give an indication about the quality of coal. Ash content may be
determined as air dried basis and on oven dried basis. The main
difference between the two is that the latter is determined after expelling
the moisture content in the sample of coal.
Coal ash includes a number of by-products produced from burning coal,
including:
Fly Ash, a very fine, powdery material composed mostly of silica
made from the burning of finely ground coal in a boiler.
Bottom Ash, a coarse, angular ash particle that is too large to be
carried up into the smoke stacks so it forms in the bottom of the coal
furnace.
Boiler Slag, molten bottom ash from slag tap and cyclone type
furnaces that turns into pellets that have a smooth glassy appearance
after it is cooled with water.
Flue Gas Desulfurization Material, a material leftover from the
process of reducing sulfur dioxide emissions from a coal-fired boiler
that can be a wet sludge consisting of calcium sulfite or calcium
sulfate or a dry powered material that is a mixture of sulfites and
sulfates.[5]
Coal ash is one of the largest types of industrial waste generated in
the United States. According to the American Coal Ash
Association's Coal Combustion Product Production & Use Survey
Report, nearly 130 million tons of coal ash was generated in 2014.
2.3. Volatile matter:
Volatile matter in coal refers to the components of coal, except for
moisture, which are liberated at high temperature in the absence of air.
This is usually a mixture of short- and long-chain hydrocarbons, aromatic
hydrocarbons and some sulfur. The volatile matter of coal is determined
under rigidly controlled standards. In Australian and British laboratories
this involves heating the coal sample to 900 5 C (1650 10 F) for 7
min.
2.4.Fixed carbon:
The fixed carbon content of the coal is the carbon found in the material
which is left after volatile materials are driven off. This differs from the
ultimate carbon content of the coal because some carbon is lost in
hydrocarbons with the volatiles. Fixed carbon is used as an estimate of the
amount of coke that will be yielded from a sample of coal. Fixed carbon is
determined by removing the mass of volatiles determined by the volatility
test, above, from the original mass of the coal sample.

P a g e | 10

Table: Proxymite analysis of typical coal:


Lignite

Bituminous coal
(Sample I)

Bituminous Coal

Indonesian
Coal

(Sample II)
Moisture (%)

50

5.98

4.39

9.43

Ash (%)
Volatile matter (%)

10.41
47.76

38.65
20.70

47.86
17.97

13.99
29.79

Fixed carbon (%)

41.83

34.69

29.78

46.79

3. Testing Materials and Procedure:


3.1.Testing Material:
Translucent Silica crucible.
Charcoal
Muffle furnace
Dryer
3.2. Procedure:
Moisture determination:

Dry the silica crucible in an oven and weigh.


Spread out mesh coal sample on the crucible.
Weigh the crucible again to find the exact mass of the sample.
Heat the crucible without any cover in the oven at about 1055oC for
1 hour.
Take out the crucible from the oven, cover it with the lid and cool.
Weigh the crucible to find the loss in weight of coal due to presence
of moisture.

Figure: Translucent Silica crucible.

P a g e | 11

Volatile Matter:
Heat a clean crucible and its lid at 90015oC for 7 minutes in muffle
furnace.
Allow the crucible and lid to cool on a metal plate for a minute and
in
desiccator for 10 minutes.
Weigh the crucible and lid together.
Put sample and weigh again to know the exact mass.
Insert the crucible with the lid on it into the furnace at 900oC and
keep
there for a period of 7 minutes.
Weigh the crucible with the lid to know the weight loss due to
expulsion of
volatile matter

Figure: Muffle furnace

Ash determination:
Follow the steps 1 to 3 of moisture determination.
Insert the open crucible in the furnace at 815oC for an hour.
Remove the crucible; allow it to cool for 10 minutes on the slab and
15 minutes in the desiccator.
Weigh the crucible to find the mass left which is the ash content of
the coal.

P a g e | 12

Charcoal (raw material)

(400 Muffle furnace for


1hour)

Weigh the crucible

Crucible (weighed)

Weigh the crucible

Muffle furnace
(750 for 1 hour

Weigh the crucible

Weigh the crucible with


charcoal

Muffle furnace
(105-110 for 1hour)

Weigh the crucible

Muffle furnace
(925 for 7 minutes)

Figure: Block diagram of the process.

4. Data and Calculation:


DATA:
Instruments (temperature)
Crucible
Crucible+ coal
Crucible+ coal (at 105)
Crucible+ coal (400)

Weight (g)
17.332
18.913
18.383
17.963

Crucible+ coal (750)


crucible+ coal(925)

17.925
17.917

Loss of weight (g)


1.581g(coal)
0.53(moisture content)
0.42(carbonaceous
matter)
.038g(ash content)
0.008( volatile matter
content)

P a g e | 13

Calculation:
Weight of the crucible: 17.332
Weight of the crucible with coal=18.913g
So, the weight of the coal= 1.581g
After drying the coal to 105 in muffle furnace, the new weight is =18.88g
Final weight of moister content = (18.913-18.383) g
=0.53g
And % free moisture content = (loss in weight/initial weight of coal) 100%
= (0.53/1.581)100%
= 33.52%
The next day the crucible with coal was heated to 400 and weight found=17.963
So the carboneous matter = (18.383-17.963) g
= 0.42g
On the third day, It was again heated to 750 for complete combustion and the
corresponding weight is=17.925g
So the ash content = (17.963-17.925) g
=0.038g
And the corresponding % Ash content= (loss in weight/ weight of coal without
moisture) 100%(dry basis)
= (0.038/0.631) 100%
=6.02%
% Ash content = (0.038/1.581) 100% (Wet basis)
=2.40%
Finally the crucible with the remaining content was heated to 925 and the
corresponding
Weight is =17.917g
And % volatile matter content = (loss in weight/initial weight of coal) 100%
= (0.008/0.533) 100%
=1.50%
Fixed carbon content=100-(free moisture in %+volatile matter in % +ash in %)
=100-(33.52%+2.40%+1.50%)
=62.58%

5. Result & Discussion:


Free moisture content=33.52%
Volatile matter content=1.50%
Ash content=6.02% (Dry basis)
Ash content=2.40% (Wet basis)
Fixed carbon=62.58%

P a g e | 14

proximate analysis of coal

33.52

62.58
1.5

2.4

moisture

volatile

ash

fixed carbon

Figure: Pie chart showing different content of coal after proximate analysis

Chart Title
60
49.119

50
40

33.52
30
20

23.61

22.29

19.629

17.51
12.33

10

7.03

5.9

3.14
0.195

0.18
0

4.4

2.4 1.5

group 1

group 2

group 3

group 5

group 7

19.629

22.29

17.51

23.61

33.52

ash

0.18

12.33

49.119

7.03

2.4

volatile

5.9

3.14

0.195

4.4

1.5

moisture

moisture

ash

volatile

Figure: Bar diagram of the experimental data from different groups.

P a g e | 15

Discussion:
The process was very much time consuming. And there was only one muffle
furnace, so we may have some fluctuation in result for this reason. But there was no
major problem occurs by our group. The crucible dont have proper cape, for this
reason some problem may happen. But we try our best to get the best possible result.

6. Conclusion:
The composition of coal varies widely and hence it is necessary to analyze and
intercept the results from the point of commercial classification. For selection of
coal for different applications is mainly made on the basis of high volatile
content, low moisture content and low ash content. The ash content of all the
samples fall within the expected range of 3-15%

Reference:
1. http://www.eia.gov/energyexplained/?page=coal_home
2. http://www.griffincoal.com.au/coal-education/coal-types/
3. http://www.renewableenergyworld.com/articles/2008/05/the-chemicalcomposition-of-coal-and-its-negative-impact-52584.html
4. https://www.scribd.com/doc/215173482/total-moisture-content-of-coal
5. https://www.epa.gov/coalash/coal-ash-basics
6.
https://www.researchgate.net/post/How_do_you_calculate_fixed_carbon_in_bio
mass

P a g e | 16

Experiment no. 02
Determination of Aniline Point of Petrol

Abstract
Aniline point is used to characterize pure hydrocarbons and to indicate aromatic content
of hydrocarbon mixtures. Our experiment covers the determination of aniline point of
petrol. Aromatic hydrocarbons exhibit the lowest values and paraffins the highest.
Cycloparaffins and olefins exhibit values that lie between those for paraffin and aromatics.
Our analysis exhibits a value of 103 that indicates the sample as paraffin.

1. Introduction:
Aniline point (AP) is a characteristic of petroleum fractions that indicates the degree of
aromaticity of hydrocarbon mixtures. Aniline point is defined as the lowest temperature
at which equal volumes of aniline and the sample become completely soluble .As amount
of aromatics in a petroleum fraction increase the aniline point decreases. Therefore, the
aniline point is a parameter that is highly related to the hydrocarbon types in petroleum
fractions. Aniline point is a useful parameter in calculation of heat of combustion, diesel
index and hydrogen content of petroleum fuels. For non-fuel products such as solvents
aniline point is usually specified to quantify their effectiveness [1].
The approximate method of testing the ignition quality of oils is based measuring the
proportion of paraffin hydrocarbons in the fuel. In the case of oils the high paraffin content
to better ignition quality. The aromatic hydrocarbons mix readily with aniline at room
temperature but mix only at relatively higher temperatures. A high aniline point indicates
a high paraffin content and higher ignition quality. Moreover aromatic hydrocarbons
dissolve natural rubber and some synthetic rubbers also. This means a higher aromatic
content in a lubricating oil otherwise it may damage the oil sealing or packing which are
usually made of rubber and used in the machines [2].

2. Theory:
The American Society for Testing Materials (ASTM) has defined aniline point as the
minimum equilibrium solution temperature for equal volumes of aniline and sample.
ASTM has also published a method for determining the aniline point by observing the
temperature at which a 50/50 mixture of oil and aniline becomes turbid upon cooling [3].
There are several methods to determinate the aniline point. These test methods cover the
determination of the aniline point of petroleum products and hydrocarbon solvents. Test
Method A is suitable for transparent samples with an initial boiling point above room
temperature and where the aniline point is below the bubble point and above the
solidification point of the aniline-sample mixture. Test Method B, a thin-film method, is
suitable for samples too dark for testing by Test Method A. Test Methods C and D are for
samples that may vaporize appreciably at the aniline point. Test Method D is particularly
suitable where only small quantities of sample are available. Test Method E describes a
procedure using an automatic apparatus suitable for the range covered by Test Methods
A and B [4].

P a g e | 17

These test methods are under the jurisdiction of ASTM Committee D02 on Petroleum
Products and Lubricants and are the direct responsibility of D02.04 on Hydrocarbon
Analysis.
It is mentionable that test method A is experimented here.
The greater the aniline point, the lower the aromatics in fuel oil. A higher aniline point
also indicates a higher proportion of paraffin. Also aniline point is used to determine the
cetane number and diesel index of fuel.
Diesel Index

aniline point

o F Degrees API gravity 60o F


100

Cetane no. =0.72*D.I + 10


Cetane number is actually a measure of a fuels ignition delay. This is the time period
between the start of injection and start of combustion (ignition) of the fuel. In a particular
diesel engine, higher cetane fuels will have shorter ignition delay periods than lower
cetane fuels
The Diesel Index indicates the ignition quality of the fuel. Diesel fuel rating based
on ignition qualities; high-quality fuel has a high index number.
Paraffin is the common name for the alkane hydrocarbons with the general formula CnH2n+2

[5]

3. Testing material and Procedures:


3.1 Material:
Petrol
Aniline
Paraffin
Thermometer
Test tube
Beaker
3.2 Procedure:
1. 3 ml of aniline and 3 ml petrol are stirred continuously in a test tube fitted with
thermometer.
2. The test tube was heated until the two merged into a homogeneous solution.
3. Heating was stopped and the tube is allowed to cool.
4. The temperature at which the two phases separate out is recorded as aniline
point.

Aniline
and Petrol
in test
tube

Heat the
mixture

Cool the
homogene
ous
solution

Record the
aniline point

P a g e | 18

Figure: Block diagram of determination of amylin point of petrol.

4. Result and Discussion:


The aniline point of the given sample is 103oC.
The thermometer fitted test tube was faulty in the experiment. There was a little bit heat
loss. Moreover, the aniline was slightly impure and the thermometer reading was faulty.
So, in the end, the experimented value was some difference, little bit fluctuated.

5. Conclusion:
Because that Point gives an approximation for the content of aromatic compounds in
the oil, since the miscibility of aniline, which is also an aromatic compound suggests
the presence of similar (i.e. aromatic) compounds in the oil. The lower the aniline point,
the greater is the content of aromatic compounds in the oil as obviously a lower
temperature is needed to ensure miscibility.
Aniline being an aromatic compound freely mixes with aromatic so a low aniline point
indicates low diesel index (because of high percentage of aromatics).
High aniline point indicates that the fuel is highly paraffinic and hence has a high Diesel
index and very good ignition quality. In case of aromatics the aniline point is low and
the ignition quality is poor.

Reference:
1. Nelson, W. L., Oil and Gas Journal, 1969, 67,122 / T. A. Albahri, M. R. Riazi
and A. A. Alqattan, Chemical Engineering Department, Kuwait University,
Octen Number and Anilne Number of Pterolium Fuels.
2. B.Tech. ENGINEERING EXP
3. Bruce B. Carr & M. S. Agruss, The Pure Oil Company, Chicago, III,
Dtetermination of the Aniline Point of Dark Petrlium Oil. /
http://pubs.acs.org/doi/abs/10.1021/i560102a002
4. ASTM Standards: D 1500 Test Method for ASTM Color of Petroleum
Products (ASTM Color Scale), For referenced ASTM standards, visit the
ASTM website, www.astm.org or contact ASTM Customer Service at
service@astm.org. For Annual Book of ASTM Standards volume information,
refer to the standards Document Summary page onthe ASTM website.
5. Niaz Salihm, University of Sulaimani, Aniline Point for Petrolium Products.

P a g e | 19

Experiment no. - 03
Determination of cloud point and pour point of the palm oil and soya bean oil
Abstract
The purpose of this experiment was to measure the pour point and cloud point of the provided oil
in the laboratory using the apparatus. The pour point of a liquid is the temperature at which it
becomes semi solid and loses its flow characteristics. In the petroleum industry, cloud point refers
to the temperature below which wax in diesel or bio wax in biodiesels form a cloudy appearance.
Through our experiment we found the cloud point of soybean and palm oil 1C and 17C
respectively and the pour point 0C and 15C respectively.

1. Introduction:
The pour point of an oil is the lowest temperature at which the oil will just flow, under standard
test conditions. The failure to flow at the pour point is usually attributed to the separation of waxes
from the oil, but can also be due to the effect of viscosity in the case of very viscous oils. Also,
particularly in the case of residual fuel oils, pour points may be influenced by the thermal history
of the sample, that is, the degree and duration of heating and cooling to which the sample has been
exposed. From a spill response point of view, it must be emphasized that the tendency of the oil to
flow will be influenced by the size and shape of the container, the head of the oil, and the physical
structure of the solidified oil. The pour point of the oils is therefore an indication, and not an exact
measure, of the temperature at which flow ceases.
In the petroleum industry, cloud point refers to the temperature below which wax in diesel or bio
wax in biodiesels form a cloudy appearance. The presence of solidified waxes thickens the oil and
clogs fuel filters and injectors in engines. The wax also accumulates on cold surfaces (e.g. pipeline
or heat exchanger fouling) and forms an emulsion with water. Therefore, cloud point indicates the
tendency of the oil to plug filters or small orifices at cold operating temperatures. In crude or heavy
oils, cloud point is synonymous with wax appearance temperature (WAT) and wax precipitation
temperature (WPT).

P a g e | 20

Biodiesel made from different feedstocks may have different cloud and pour points:

Biodiesel Feedstock

Cloud Point
(degrees Celsius)

Pour Point
(degrees Celsius)

Soybean oil

Canola oil

-9

Palm oil

17

15

Jatropha oil

Tallow

12-17

2. Theory:
Cloud point and pour point are important properties of oil. Pour point is the temperature at
which the oil ceases to flow when cooled. Cloud point is an index of dissolved wax
concentration and may be defined as the temperature at which cloudiness appears due to
separation of wax.
We used pour point apparatus to measure both pour and cloud point.

3. Materials:
1.Pour point apparatus
2.Thermometer
3.Ice
4.Palm oil and soybean oil
5. Nacl salt
6.Test tube with cork

4. Procedure:
1. The sample oil was taken in a test tube, A cork carrying the test thermometer was used to
close the test tube.
2. Then the pour point apparatus chamber was filled with crushed ice and NaCl.
3. The test tube was placed in this chamber and observed for a temperature interval of 1C.
4. When the sample became cloudy, the temperature was noted down. It is the cloud point.
5. As the process further continued, the test tube was removed and tilted to check for surface

P a g e | 21

movement. When the specimen did not flow when tilted, the tube was held horizontally for 5 sec.
If it does not flow, the corresponding temperature was taken as the pour point temperature.

Chamber
filled with
ice+ Nacl

Taking sample
oil in test tube

Putting test
tube in
chamber

Oil become
cloudy. Waxy

Oil lost fluidity

Figure: Block diagram of the procedure.

5. Result and Discussion:


The cloud point of soybean oil through our experiment was found to be 1C and the pour point to
be 0C. Actual cloud point and pour point of soybean oil is -9C and -16C respectively. So, our
measured value was far away from the actual value. This happened because the sample provided
in the laboratory might contain some impurities. Besides this the performance of the apparatus
was below the mark.

6. Conclusion:
For pumping and handling purposes, it is often necessary to know the minimum temperature at
which a particular fuel oil loses its fluid characteristics. This information can be of considerable
importance, because wide variations in pour point exist between different oils even between
oils of comparable viscosity.
The behavior of an oil at low temperature depends upon the type of crude from which it is

P a g e | 22

refined, the method of refining and the presence, if any, of additives. Paraffinic base stocks
contain waxy components which remain in solution at warmer temperatures. When the
temperature is decreased, these waxy components begin to crystallize. They become fully
crystallized at a temperature slightly below the pour point. At this temperature, the undisturbed
oil generally will not flow under the influence of gravity.

References:
1. https://en.wikipedia.org/wiki/Pour_point
2. https://en.wikipedia.org/wiki/Cloud_point
3. http://www.oilproduction.net/files/Introduction.pdf
4.https://www.eagle.org/eagleExternalPortalWEB/ShowProperty/BEA%20Repository/Rules&G
uides/Current/31_HeavyFuelOil/Pub31_HeavyFuelOil

P a g e | 23

Experiment no. 04
Determination of Flash point and Fire point of Kerosene oil

Abstract:
The flash point of a volatile material is the lowest temperature at which vapors of the material
will ignite, given an ignition source. Flash point measuring requires an ignition source. At flash
point, the vapor may not be burn if the ignition source is removed.
The fire point of a fuel is the lowest temperature at which the vapour of that fuel will continue to
burn for at least 5 seconds after ignition by an open flame. Fire point may be considered as the
lowest temperature of the liquid at which vapor combustion and burning commences. A fire
point happens when an ignition source is applied and the heat produced is self-sustaining, as it
supplies enough vapors to combine with air and burn even after the removal of the ignition
source.

1. Introduction:
Flash point is a temperature and the property of a volatile material which suggests when volatile
material gives off sufficient vapor when heated, it will start ignite for a moment but not lasts
more than few seconds. But in fire point the material will produce a flame for at least 5 seconds
from the ignition point.
The flash point and fire point of fuel is very important to know as it is essential for determining
the methods for transporting and handling the fuel accordingly. Flash point and fire point help in
determining the nature of fuel's Flammability. Lower value of flash point means fuel is highly
flammable.

2. Theory:
The flash point test can be summarized as a procedure in which a test specimen is introduced
into a temperature-controlled test cup and an ignition source is applied to the vapors produced by
the test specimen. The aim of the test is to determine whether the vapor/air mixture is flammable
or at what temperature the vapor/air mixture is flammable.
It is important to realize that the value of the flash point is not a physical constant but is the result
of a flash point test and is dependent on the apparatus and procedure used.
There are two general classes of flash point tests: open cup and closed cup.
We used closed cup method in our laboratory.

P a g e | 24

3. Testing materials and procedures:


Materials:
1.
2.
3.
4.
5.

Flash point apparatus


Thermometer
Bunsen Burner
Gasoline (Petrol)
Stirrer

Procedure:
1. We took kerosine sample in the brass cup of the apparatus
2. The sample is heated and stirred at a specific rates
3. An ignition source is directed into the cup at regular intervals with simultaneous
interruption of the stirring.
4. When the vapor caught fire the temperature was noted as flash point.
5. We continued the process and when the oil vapor caught fire and continued to fire, the
temperature was noted as fire point.

Taking
Patrol oil in
the
apparatus

Heating &
Stirring

Directing
ignition
source

Appearance
of flash
point

Figure: Flow diagram of experimental process.

Apparance
of fire
point

P a g e | 25

4. Result & Discussion:

5. Conclusion:
The flash point and fire point are empirical measurements. The test methods we used is
applicable for relatively nonvolatile or nonflammable materials to assessing the overall
flammability hazard. This method is also used for product specifications and regulations due to
its better precision.

References:
1.
2.
3.
4.

https://en.wikipedia.org/wiki/Flash_point
https://en.wikipedia.org/wiki/Fire_point
http://blog.anton-paar.com/a-guide-to-flash-and-fire-point-measurement/
http://www.mechanicalduniya.com/2012/01/importance-of-flash-point-fire-point.html

P a g e | 26

Experiment no. - 05
Determination the kinematic viscosity of transparent and opaque liquid

Abstract
Viscosity is a property of a liquid and is defined as the resistance of a liquid to flow. The purpose
of this experiment is to determine the kinematic viscosity. A kinematic viscometer is used to
measure the flow of soybean oil. Kinematic viscosity is determined by kinematic viscometer
with help of its constants. The viscosity of liquid found at temperature 40. The liquid samples
taken such a way in that are low sticky.

1. Introduction
The viscosity of a fluid is measure of its resistance to gradual deformation by shear stress or
tensile stress. For liquids, it corresponds to the informal concept of thickness. For example
engine oil has much higher viscosity than water. Viscosity is a property arising from collisions
between neighboring particles in a fluid that are moving at different velocities. When the fluid is
forced through a tube, the particles which comprise the fluid generally move more quickly near
the tubes axis and more slowly near its wall; therefore some stress (such as a pressure difference
between the two ends of the tube), is needed to overcome the friction between particle layers and
keep the fluid moving. For the same velocity pattern, the stress required is proportional to the
fluids viscosity. A fluid has no resistance to shear stress is known as an ideal fluid. Zero
viscosity is observes only at low temperature, in super fluids. Otherwise all fluids have positive
viscosity, and are technically said to be viscous or viscid fluid. Fluid flow plays a very important
part in the processing of materials. Most processes are based on the use of fluids either as raw
materials, reagents, or heat transfer media. A liquid in a state of steady flow on a surface may be
supposed to consist of series of parallel layers moving one above the other. If any two layers of
liquid moves with different velocities, the top layer moves faster than next layer due to viscous
drag. If viscosity of oil is too low, then a liquid oil film cant be maintained between two moving
parts or sliding surfaces and consequently excessive wear and tear will take place, on other hand
if viscosity is too high it will results in excessive friction. [1]
Viscosity is a measure of the resistance of a fluid which is being deformed by either shear stress
or tensile stress. In everyday terms (and for fluids only), viscosity is "thickness" or "internal
friction". Thus, water is "thin", having a lower viscosity, while honey is "thick", having a higher
viscosity. Put simply, the less viscous the fluid is, the greater its ease of movement (fluidity).[2]
In general, in any flow, layers move at different velocities and the fluid's viscosity arises from
the shear stress between the layers that ultimately opposes any applied force. The relationship
between the shear stress and the velocity gradient can be obtained by considering two plates
closely spaced at a distance y, and separated by a homogeneous substance. Assuming that the
plates are very large, with a large area A, such that edge effects may be ignored, and that the

P a g e | 27

lower plate is fixed, let a force F be applied to the upper plate. If this force causes the substance
between the plates to undergo shear flow with a velocity gradient u (as opposed to just shearing
Elastically until the shear stress in the substance balances the applied force), the substance is
called a fluid. The applied force is proportional to the area and velocity gradient in the fluid and
inversely proportional to the distance between the plates. Combining these three relations results
in the equation:

Where is the proportionality factor called viscosity.

Laminar shear, the non-constant gradient, is a result of the geometry the fluid is
flowing through (e.g. a pipe). [3]

Laminar shear of fluid between two plates. Friction between the fluid and the moving
Boundaries causes the fluid to shear. The force required for this action is a measure of
The fluid's viscosity. This type of flow is known as a Couette flow.[4]

P a g e | 28

1.1. Types of viscosity


Newton's law of viscosity, given above, is a constitutive equation (like Hooke's law, Fick's law,
Ohm's law). It is not a fundamental law of nature but an approximation that holds in some
materials and fails in others. Non-Newtonian fluids exhibit a more complicated relationship
between shear stress and velocity gradient than simple linearity. Thus there exist a number of
forms of viscosity:
Newtonian: fluids, such as water and most gases which have a constant viscosity.
Shear thickening: viscosity increases with the rate of shear.
Shear thinning: viscosity decreases with the rate of shear. Shear thinning liquids are very
commonly, but misleadingly, described as thixotropic.
Thixotropic: materials which become less viscous over time when shaken, agitated, or
otherwise stressed.
Rheopectic: materials which become more viscous over time when shaken, agitated, or
otherwise stressed.
A Bingham plastic is a material that behaves as a solid at low stresses but flows as a viscous
fluid at high stresses.
A magnetorheological fluid is a type of "smart fluid" which, when subjected to a magnetic
field, greatly increases its apparent viscosity, to the point of becoming a viscoelastic solid.

Viscosity, the slope of each line, varies among materials [5]

P a g e | 29

1.2.Viscosity coefficients
Viscosity coefficients can be defined in two ways:
Dynamic viscosity, also absolute viscosity, the more usual one (typical units Pas, Poise, P);
Kinematic viscosity is the dynamic viscosity divided by the density (typical units m2/s,
Stokes, St).
Viscosity is a tensorial quantity that can be decomposed in different ways into two independent
components. The most usual decomposition yields the following viscosity coefficients:
Shear viscosity, the most important one, often referred to as simply viscosity, describing the
reaction to applied shear stress; simply put, it is the ratio between the pressure exerted on the
surface of a fluid, in the lateral or horizontal direction, to the change in velocity of the fluid as
you move down in the fluid (this is what is referred to as a velocity gradient).
Volume viscosity (also called bulk viscosity or second viscosity) becomes important only for
such effects where fluid compressibility is essential. Examples would include shock waves and
sound propagation. It appears in the Stokes' law (sound attenuation) that describes propagation of
sound in Newtonian liquid. Alternatively,
Extensional viscosity, a linear combination of shear and bulk viscosity, describes the reaction
to elongation, widely used for characterizing polymers. For example, at room temperature, water
has a dynamic shear viscosity of about 1.0 . 103 Pas and motor oil of about 250 . 103 Pas.[6]
1.3. Calculations:
Calculate the kinematic viscosity as follows:
Kinematic viscosity. cSt = Ct
Where:
C = calibration constant of the viscometer, cSt/s, and
t = flow time, s
2. Experimental
2.1. Materials:
1. Kinematic viscometer
2. Soybean oil
3. Timing device
4. Temperature measuring device
5. Ostwald viscometer

Fig: Kinematic viscometer

P a g e | 30

2.2. Methods:
1. Ascertain that the thermometer has been standardized recently; new thermometers may require
checking every week.
2. Maintain the bath at the test temperature. Apply the necessary corrections, if any, to all
thermometer readings.
3. Select a clean, dry, calibrated viscometer which will give a flow time not less than the
minimum specified for the viscometer, or 200s, whichever is the greater.
4. Charge the viscometer in the manner dictated by the design of the instrument, this operation
being in conformity with that employed when the instrument was calibrated.
5. Allow the charged viscometer to remain in the bath long enough to reach the test temperature.
Because this time will vary for the different instruments and for different temperatures, establish
a safe temperature equilibrium time by trial. Where the design of the viscometer requires it,
adjust the volume of the test sample after the sample has reached temperature equilibrium.
6. Use suction (if the sample contains no volatile constituents) or pressure to adjust the head
level of the test sample to a position in the capillary arm of the instrument about 5mm ahead of
the first timing mark.
7. With the sample flowing freely, measure in seconds, to within 0.2s, the time required for the
meniscus to pass from the first timing mark to the second. If this flow time is less than the
specified minimum, select a viscometer with a capillary of smaller diameter and repeat the
operation.
3.Results and Discussion:
The flow time, t = 37.33 min = (37.33*60) s = 2239.8s
Kinematic viscosity, cSt = Ct = (0.0208652 mm2/s2)*(2239.4s) = 46.74 mm2/s
So, the kinematic viscosity of the soybean oil is 46.74 mm2/s

4.Conclusion:
Accurate measurements of viscosity are essential in engineering calculations and design of
equipment that move liquids, such as pumps, pipes and valves. My experiment shows that effect
of temperature on a liquid's viscosity must be taken into account in the design calculations
5.Reference:
[1] DOI: 10.15680/IJIRSET.2015.0404020
[2] Symon, Keith (1971). Mechanics (Third ed.). Addison-Wesley. ISBN 0-201-07392-7.
[3]

http://en.wikipedia.org/w/index.php?title=File:Laminar_shear_flow.svg

[4]

http://en.wikipedia.org/w/index.php?title=File:Laminar_shear.svg

[5]

http://en.wikipedia.org/w/index.php?title=File:Viscous_regimes_chart.png

P a g e | 31

Experiment no. - 06
Determination of calorific value of a fuel (ethanol) by using bomb calorimeter.

Abstract:
There are many criterias for selecting a fuel like as calorific value, calorific intensity,
flame temperature, moisture content, ash content etc. Calorific value is one of them. The
objectives of this experiment is to determine the calorific value of ethanol. Here, we determine the
calorific value of a solid or liquid fuel by high pressure oxygen bomb calorimeter. The value of
the calorific value of the fuel is 26120.74 j/g. Our experimental the calorific value of ethanol was
found to be close to the standard value.

1. Introduction:
Calorimetry is the science of measuring quantities of heat, as distinct from temperature. The
instruments used for such measurements are known as calorimeters. In this publication we are
concerned only with oxygen bomb calorimeters, which are the standard instruments for
measuring calorific values of solid and liquid combustible samples.
The calorific value (heat of combustion) of a sample may be broadly defined as the number of
heat units liberated by a unit mass of a sample when burned with oxygen in an enclosure of
constant volume. In this reaction the sample and the oxygen are initially at the same temperature
and the products of combustion are cooled to within a few degrees of the initial temperature; also
the water vapor formed by the combustion is condensed to the liquid state. A more exact
definition would specify the temperature at which the reaction begins and ends. However, the
change in the heat of combustion with possible variations in the initial temperature is so small
that this specification is not necessary. Also, the initial and final temperatures are not the same
differing by the amount of temperature rise in the calorimeter but the effect of this difference is
small and usually it is neglected. Thus the term calorific value (or heat of combustion) as
measured in a bomb calorimeter denotes the heat liberated by the combustion of all carbon and
hydrogen with oxygen to form carbon dioxide and water, including the heat liberated by the
oxidation of other elements such as sulfur which may be present in the sample.
The heat energy measured in a bomb calorimeter may be expressed either as calories (cal),
British thermal units (Btu) or Joules (J), with the International Steam Table calorie as the basic
unit in this system.

P a g e | 32

Fig: bomb calorimeter

2. Theory:
The calorific value of a fuel is defined as the amount of heat obtainable by the complete
combustion of a unit mass of the fuel. There are two types of calorific value.
1. The gross calorific value
2. The net calorific value.
Gross calorific value (GCV) represents the absolute value of the specific energy of combustion,
in joules, for unit mass of a solid biofuel burned in oxygen in calorimetric bomb under the
conditions specified. On the basis of the GCV and the elemental composition, the net calorific
value (NCV) is calculated.
Net C.V = Gross C.V- Latent heat of water vapor, formed during the combustion of m grams of
the fuel.
Here we use heat exchanging method by transferring heat of combustion of fuel to water.

P a g e | 33

Heat exchange between the solid and fluid is said to occur due to convection whenever there is a
difference in temperature between two phases and there is motion in the fluid. If the motion of
the fluid is caused by the buoyancy forces which arise due to variation in the density of the fluid
with temperature, the process is called free or natural convection. If the motion of the fluid is
caused by external means such as blower, wind, fan or pump, the process is called as forced
convection. Heat exchange due to convection may be described in terms of a heat transfer
coefficient h by Newtons law of cooling as:
Q = Ah (1 2 )
A is the area of the solid-fluid interface, T1 and T2 are the solid and fluid temperatures
respectively.
Weight of the fuel sample taken = m kg
Gross calorific value of the fuel = j/kg
Weight of water taken in the calorimeter = W1 kg
Weight of the calorimeter (i.e. bucket) = W2 kg
Initial temperature = t1
Final temperature = t2
Heat liberated by the combustion of fuel = m j
Specific heat capacity of calorimeter(i.e. bucket made of stainless steel), Cs = 450 j/kg
Specific heat capacity of water, Cw = 4200 j/kg
Heat liberated = Heat absorbed
m = W1Cw(t2-t1) + W2Cs(t2-t1)
W1Cw(t2t1) + W2Cs+(t2t1)

3. Equipment:
1. Bomb
2. Stirrer
3. Calorimeter
4. Thermometer
5. Ethanol (1.5g)

(1)

P a g e | 34

4. Procedure:
The testing procedure conforms to the ASTM d4809 standard.
1) We took the bomb out of the calorimeter, opened the bomb, and took the crucible out.
2) We took 0.4 grams of the fuel sample in the crucible and place it in the holder of the bomb.
3) Then we took about 15-20 cm fuse wire and set it in a manner that it touches the fuel sample
or is immersed in it.
4) We closed the bomb tightly and then using an oxygen cylinder, filled the bomb with
oxygen. The pressure was about 20 atm. After filling with oxygen, we let all the air out
through the valve to purge all the nitrogen in the bomb. Then again fill the bomb with
oxygen of 20 atmospheres approx.
5) We took 1.64 liters of water by carefully measuring and put the water in the bucket of the
calorimeter.
6) Then we put the bomb in the bucket of the calorimeter and ensured that it was fully
immersed in the water.
7) Then, we attached the two electrodes with the bomb and turned on the stirrer.
8) We noted down the temperature of the calorimeter before ignition.
9) After that, we plugged in the electrodes plug in a socket and switched it on. Then we turned
it off after a few seconds.
10) Afterwards we saw the temperature rise gradually and noted down the maximum
temperature.
11) After finishing the experiment, we washed the bomb and the bucket so there is no residue
of burned fuel or wire.

5. Calculation:
Weight of the sample, m = 0.4*10-3 kg
Initial temperature, t1 = 33.52
Final temperature, t2 = 34.95
Weight of water taken in the calorimeter, W1 = 1.64 kg
Weight of the calorimeter (i.e. bucket), W2 = 0.93kg

P a g e | 35

Putting all the values in equation (1), we get,


=

{1.64 4200 (34.95 33.52)} + {0.93 450 (34.95 33.52)}


0.4 10^ 3

= 26120.74*103 j/kg
= 26120.74 j/g
So, the Gross calorific value of ethanol is 26120.74 j/g

6. Result & Discussion:


The Gross calorific value of ethanol is 26120.74 j/g
Actual gross calorific value of ethanol is 29700 j/g. Reasons for the deviation in value are.Here we
got the value of calorific value of ethanol without considering fuse wire correction, cotton thread
correction , cooling correction. Again we did not consider the weight of calorimeter, bomb,
thermometer, stirrer etc for lacking of data of them. In another way motor did not work so that we
had to done this experiment without stirrer. Again we have to assume that all fuel is burning up
but actually some fuel exist after the final temperature .So that another error does not include in
the calculation. But finally we get a calorific value of ethanol fuel.

References:
1. A Textbook of Engineering Chemistry by Dr. S.S. Dara , Dr. S.S.Umare
2. Wikipedia
3. A journal paper CALORIFIC VALUE DTERMINATION OF SOLID BIOMASS FUEL BY
SIMPLIFIED METHOD by Giuseppe Toscano, Ester Foppa Pedretti.