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Chemical Engineering Department

Faculty of Materials and Chemical Engineering
Lab Manual
CH252 Chemical Lab
Energy engineering

Submitted to:
Sir umar
Submitted by :
Zainab tariq
2019555
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TABLE OF CONTENTS
SERIES NAME OF EXPERIMENTS PAGE
NO
1 Cloud point of petroleum products 03
2 Pour point of petroleum products 05
3 Flash point of petroleum products 08
4 Fire point of petroleum products 11
5 Conradson carbon residue of petroleum products 12
6 Softening point of petroleum products 14
7 Aniline point of petroleum products 15
8 Penetration of petroleum products 18
9 Proximate analysis of coal 20
A) Percentage of moisture contents 21
b) Percentage of ash contents 21
c) Percentage of volatile matter 22
d) Percentage of fixed carbon 24
10 Specific gravity of petroleum products
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Cloud Point of Petroleum Products

Objective:
To calculate the cloud point of petroleum products
Theory:
Cloud point is the temperature at which wax (paraffin) begins to separate when oil
chilled to a low temperature, and it serves as an important indicator of practical
performance in automotive applications in low temperatures. he cloud point of a
detergent is the temperature at which a detergent solution passes from an isotropic
micellar system into a two-phase system. This property of a detergent has been
employed in purification methodologies. Bordier extracted proteins from a lipid
bilayer by creating a two-phase system with Triton X-114, which has a cloud point
of 22°C [29]. This detergent separates into an aqueous phase and a detergent phase
at 30°C and integral membrane proteins will be preferentially found in the
detergent phase while hydrophilic proteins show up in the aqueous phase. The
solution shows clouding-like nonionic surfactants above 25°C and near the
equimolar point. In a mixed solution, both surfactants stoichiometrically exist as
1:1 ionic-bonded ion pairs.

Applications of Cloud Point:

The applications of cloud point extraction (CPE) methodology for separation and
preconcentration of different substances including metal ions, nano-particles and
organic molecules. The CPE as any extraction procedure separates the analyte
from whole sample into small volume to increase the sensitivity of analysis and to
eliminate effect of interference from sample background. The major features of
CPE technique over the other separation methods are effectiveness, rapidness,
simplicity and safety. It minimizes or ignores the utilization of toxic organic
solvents and therefore the procedure is termed as “eco-friendly tool”. In the present
review, the application of CPE in the determination of wide range of analytes was
discussed with special concern to recent developed procedures. The main
advantages and limitations of the technique were also provided.

Freezing Point:
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The freezing point is the temperature at which the liquid solvent and solid solvent
are at equilibrium, so that their vapour pressures are equal. When a non-volatile
solute is added to a volatile liquid solvent, the solution vapour pressure will be
lower than that of the pure solvent. he freezing point is lower than the melting
point in the case of mixtures and for certain organic compounds such as fats. As a
mixture freezes, the solid that forms first usually has a composition different from
that of the liquid, and formation of the solid changes the composition of the
remaining liquid, usually in a way that steadily lowers the freezing point. This
principle is used in purifying mixtures, successive melting and freezing gradually
separating the components.

Procedure:
 To modify the temperature of set point on the digital thermo regular hold
arrow down key. The display will show the actual temperature and sp1. Now
it is possible to enter set point value by pressing arrows. The value will be
stored automatically after some seconds or press P to confirm immediately.
 Bring the sample to a temperature at least 14 degree above the approximate
cloud point.
 Remove any moisture present by a method such as filtration through dry
lintels filter paper until the oil is perfectly clear, but make such filtration at a
temperature of atleast 14 degree above the approximate cloud point.
 Pour the sample into the test jar to the level mark.
 Close the test jar tightly with cork carrying temperature. the thermometer
and the jar are coaxial and the thermometer bulb is resting on the bottom of
the jar.
 If the expected cloud point is above -36 degree use the high cloud pour point
thermometer and the low cloud and pour point the thermometer if the
expected cloud point is below -36 degree.
 To avoid the frost formation which may cause erroneous results see that the
disk and the distance ring and the inside of the jacket are clean and dry.
 Place the disk in the bottom of the jacket the use of jacket cover while the
empty jacket is cooling is permitted.
 Insert the test jar in the jacket.
 Maintain the temperature of the cooling bath at 0 to 1.5 degree.
 At each test thermometer reading that is a multiple of 1 degree remove the
test jar from the jacket quickly and without disturbing the sample, inspect
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cloud point and replace cloud point and replace the jacket,. This operation
shall not require more then 3 seconds.
 Report the cloud point to the nearest 1 degree at which any cloud is observed
at the bottom of the test jar , which is confirmed by continued cooling.

Observations:
Repeat the experiment 3-4 times and note down the readings.

Results:
Cloud point of the given sample is :0 degree of diesel
Palm oil:-10 degree

Pour Point of Petroleum Products:

Objective:
To calculate the pour point of petroleum products
Theory:
Pour point is defined as the lowest temperature at which the test fluid can be
poured under the prescribed test conditions. It is one of the properties that
determine the low temperature fluidity of a lubricating oil. Paraffinic base oils are
widely employed in various lubricant applications for their oxidation stability,
oxidation resistance, and good viscosity index. These oils are derived from crude
oils through different refining process and contain saturated hydrocarbon
molecules with a distribution of carbon chain lengths. The linear and very lightly
branched hydrocarbons, considered as waxy materials, crystallize out of solution as
temperature decreases, leading to a hazy appearance. The temperature at which this
happens is defined as the cloud point(ASTM Standard D2500) of the oil and can be
measured by ASTM D2500. As the temperature is lowered further, additional wax
molecules precipitate; the wax crystals start to grow into plates.
Pour Point Depressants:
Pour point depressants are used to allow the use of petroleum based mineral oils at
lower temperatures. The lowest temperature at which a fuel or oil will pour is
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called a pour point. Wax crystals, which form at lower temperatures, may interfere
with lubrication of mechanical equipment. Pour Point Depressants act as a wax
crystal modifier. Modification is achieved by nucleation, co-crystallization and
anti-agglomeration, which results in reduction of the size and shape of wax
crystals. Wax-crystals are not inhibited but modified in a way that they do not
precipitate.
Applications of Pour Points:
Pour Point Depressants act as a wax crystal modifier. Modification is achieved by
nucleation, co-crystallization and anti-agglomeration, which results in reduction of
the size and shape of wax crystals. Wax-crystals are not inhibited but modified in a
way that they do not precipitate. Pour point depressants are used to allow the use of
petroleum based mineral oils at lower temperatures. The lowest temperature at
which a fuel or oil will pour is called a pour point. Wax crystals, which form at
lower temperatures, may interfere with lubrication of mechanical equipment.
Procedure:
 To modify the temperature of set point on the digital thermo regular hold
arrow down key. The display will show the actual temperature and sp1. Now
it is possible to enter set point value by pressing arrows. The value will be
stored automatically after some seconds or press P to confirm immediately.
 Pour the specimen into the test jar to the level of mark. When the necessary
heat the specimen in a water bath until its just sufficiently fluid to pour into
the test jar.
 Close the test jar with the cork carrying the high pour temperature. See that
the thermometer and the jar are coaxial and the thermometer bulb is
immersed so the beginning of the capillary tube is 3mm.
 For the measurement of the pour point, subject the specimen in the test jar to
the following preliminary treatment
 Sample having pour point below -33
 Samples having pour point of -33 and above
 Clean and dry the disk and the inside of the jacket to avoid the frost
formation which may cause erroneous results.
 Place the disk in the bottom of the jacket. Place the distance ring around the
test jar 25mm form the bottom. Insert the test jar with distance ring in the
jacket.
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 If the specimen in the jar does not flow when tilted hold the jar in a
horizontal position for 5 seconds and observe carefully. If the specimen
shows any movement replace the test jar immediately in the jacket and
repeat a test for flow at the next temperature.
 Determine the lower and upper temperature.
 For lower point heat the sample while stirring to 105 and pour it into the jar.
 Add 3 degree to the temperature recorded and the result as the pour point.
Observations:
Repeat the experiments for 3-4 times for the perfect point to attain.
Results:
The pour of the given sample diesel is -20 degree
And that palm oil is -29 degree

Flash Point and Fire Point of Petroleum Products:

Objective:
To calculate the flash point and fire point of the petroleum products.
Theory:
Flash point is the lowest temperature at which a chemical can vaporize to form an
ignitable mixture in air. A lower flash point indicates higher flammability.
Measuring a flash point (open-cup or close-cup) requires an ignition source. At the
flash point, the vapor may cease to burn when the ignition source is removed. The
observed temperature when the flame momentarily ignites the vapor/air mixture is
the Flash Point. The ignitions repeat as the liquid temperature continues to rise.
The observed temperature when the burning becomes continuous is the Fire Point.
Principle of Operation:
The flash point is the lowest temperature at which a volatile substance evaporates
to form an ignitable mixture with air in the presence of an igneous source and
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continues burning after the trigger source is removed. The flash point of a solvent
has no direct effect on its capability as a cleaning solvent. It does, however, have a
dominant indirect effect on selection of the cleaning process, cleaning equipment,
and cleaning procedures, as well as packaging, transportation, selection, and
disposal. In other words, specifications for the above issues all incorporate flash
point. Other than solvency, there is no more important parameter than flash point
in solvent cleaning. The flash point is an important concept in fire investigation
and fire protection because it is the lowest temperature at which a risk of fire exists
with a given liquid. It is crucial in many circumstances to establish the presence of
some liquids and to know their flash point during the investigation process. Flash
points usually are found in the literature. MSDS8 are particularly good resources
for flash point values of commercial chemicals and products. As a general rule for
hydrocarbons, the simpler the molecule, the lower the flash point. Although some
equations have been developed to calculate flash point, their utility is limited due
to significant variations in their accuracy.
Fire point:
Fire point refers to the temperature at or above which a flammable liquid produces
enough vapor to ignite by spark or flame and burn for at least five seconds. The
fire point is usually 10°C more than the flash point of a liquid. The fire point is the
temperature at which lubricant combustion will be sustained. The flash and fire
points are useful in determining a lubricants volatility and fire resistance. A
lubricant exhibiting a flash point significantly lower than normal will be suspected
of contamination with a volatile product. Fire is the rapid oxidation of a material in
the exothermic chemical process of combustion, releasing heat, light, and various
reaction products. The flame is the visible portion of the fire. Flames consist
primarily of carbon dioxide, water vapor, oxygen and nitrogen.
Flammable limits:
The minimum and maximum concentration of fuel vapor or gas in a fuel vapor or
gas/gaseous oxidant mixture (usually expressed in percent by volume) defining the
concentration range (flammable or explosive range) over which propagation of
flame will occur on contact with an ignition source. The lower flammability limit
(LFL) identifies the smallest mixture able to sustain a flame. The upper flammable
limit (UFL) identifies the richest flammable mixture. A quantifiable difference
exists between the flammability limit and explosive limit. Atmospheres with a
concentration of flammable vapors at or above 10 percent of the lower explosive
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limit (LEL) are considered hazardous when located in confined spaces. However,
atmospheres with flammable vapors below 10 percent of the LEL are not
necessarily safe. Such atmospheres are too lean to burn.
Ignition temperature:
The ignition temperature of a substance is the least temperature at which the
substance starts combustion. Substances which spontaneously ignite in a normal
atmosphere at naturally ambient temperatures are termed pyrophoric. The most
commonly known flammable liquid is gasoline. It has a flash point of about -50° F
(-65° C). The ignition temperature is about 495° F (232(232° C) [sic], a
comparatively low figure."
Difference between open cup and closed cup :
Open cup flash point is the flash point we obtain from open cup method where the
vapour above the liquid is in equilibriums with the liquid. In contrast, closed cup
flash point is the flash point we obtain from the closed cup method where the
vapour above the liquid is not in equilibrium with the liquid. Closed cup testers
normally give lower values for the flash point than open cup (typically 5–10 °C or
9–18 °F lower) and are a better approximation to the temperature at which the
vapour pressure reaches the lower flammable limit. ... Methods for determining the
flash point of a liquid are specified in many standards.
Applications:
Flash point testing is a procedure designed to determine whether a sampled
mixture of vapour and air is flammable. It can also determine the temperature at
which flammability occurs in a sample. The lowest temperature at which its
vapours ignite from an ignition source is the flash point of a material. "Flash point"
means the minimum temperature at which a liquid gives off vapor within a test
vessel in sufficient concentration to form an ignitable mixture with air near the
surface of the liquid, and shall be determined as follows: (a)(14)(i) For a liquid
which has a viscosity of less than 45 SUS at 100 deg.
Cleveland Open Cup Flash Point Tester:
The Cleveland open-cup method is one of three main methods in chemistry for
determining the flash point of a petroleum product using a Cleveland open-cup
apparatus, also known as a Cleveland open-cup tester. First, the test cup of the
apparatus (usually brass) is filled to a certain level with a portion of the product.
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Used to determine flash point of petroleum products and bituminous materials,

excepting fuel oil and materials having a flash point of lower than 79°C.
Procedure:
Flash Point Testers measure and determine the lowest point at which a test
sample’s temperature and vapor pressure become ignitable in air. A sample is
placed inside the test cup and heated at a precise rate. A test flame is then passed
across the cup to determine the lowest temperature at which the vapor will ignite.
After the flash point has been established and recorded continue heating the oil at
the specified rate of 5 to 6 degree per minute and apply the test flame at the same
intervals I e every 2 degree until the oil ignites and continues to burn for a period
of atleast five seconds. The temperature readings at the time of the flash point
application that caused burning for a period of 5 seconds or more is the fore point.
Observations:
Repeat the experiment 3 to 4 times
Result:
The fire point of diesel fuel is: 69 degree Celsius
The flash point of diesel fuel is: 76 degree Celsiu

CONRADSON CARBON RESIDUE OF PETROLEUM PRODUCTS

Objective:
It covers the determination of the amount of carbon residue left after evaporation
and pyrolysis of an oil, and is intended to provide some indication of relative coke
forming properties. This test method is generally applicable to relatively non-
volatile petroleum products which partially decompose on distillation at
atmospheric pressure.
Theory:
Carbon residue is defined as the residue formed by evaporation and thermal
degradation of a carbon containing material. This test is used to designate the
carbonaceous residue formed after evaporation and pyrolysis of a petroleum
product under the conditions specified.

Apparatus used:
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1. Porcelain crucible
2. Skidmore iron crucible
3. Spun sheet iron crucible
4. Wire support
5. Hood
6. Insulator
7. Burner

Procedure:
A weighed quantity of sample is placed in a crucible and subjected to destructive
distillation. The residue undergoes cracking and coking reactions during a fixed
period of severe heating. At the end of the specified heating period, the test
crucible containing the carbonaceous residue is cooled in desiccators and weighed.
The residue remaining is calculated as a percentage of the original sample, and
reported as Conradson carbon residue.
Results:
 Sample mass used: 106 grams
 Mass of carbon residue: 84.8 grams
 Carbon residue: 84.6*100/106=79.8%

SOFTENING POINT OF PETROLEUM PRODUCTS

OBJECTIVE:
To introduce a method of testing to determine the softening point of bituminous
binder by ring and ball method.
THEORY:
The softening point is the temperature at which a material softens beyond some
arbitrary softness which the ring and ball test is used to determine the softening
point of bitumen, asphalt and coal tar. The softening point is useful in the
classification of bitumen
EQUIPMENT USED:
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1. A brass shouldering ring

2. A steel ball
3. Ball centering guide
4. Ring holder
5. Brass pouring plate
6. Water bath and thermometers
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PROCEDURE:
 Take the bitumen sample in a vessel and heat it to a temperature of 75-
100°C- above its approximate softening point. Allow the bitumen to melt
until it is converted completely into a liquid state. Stir the bitumen if
necessary, so that it is melted completely and is free from air bubbles and
water. If the need arises, filter it through IS sieve 30.
 Prepare a mixture of glycerine and dextrine in equal proportions. Mix it
well. Then coat the surface of the metal or glass plate. This prevents the
bitumen from sticking to the plate.
 Heat the rings to approximately same temperature as that of the molten
bitumen and place them on the glass or metal plate coated with the mixture
of glycerine and dextrine.
 Pour the molten bitumen in the rings carefully till the rings are slightly filled
above the top level.
  Allow the rings to cool at room temperature in air for 30 minutes.
 Cut the excess bitumen on the surface with the help of hot, straight-edged
putty knife or spatula and level the top surface.

CALCULATIONS:
1. Softening point of the given sample (when ball drops down from first
ring) =68.5 degree
2. Softening point of the given sample (when ball drops down from the first
ring) =69.0 degree
3. (Average) Softening point of the given sample =68 degree

CONCLUSION:
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By performing the softening point test of bitumen, we can determine whether the

given bitumen sample meets the specification requirements for softening point as
given in the standards.The softening value found out by the practical is compared
to the standard value and thus it can be concluded whether the sample meets the
softening point criteria.Softening point is one of the measures of the quality of
bitumen along with other measures such as penetration, ductility value, and so on.

ANNILINE POINT OF PETROLEUM PRODUCTS

Objective:

To determine the aniline of petroleum products and hydrocarbon solvents.

Requirements: Aniline point apparatus, Thermometer, Electric heating device,
pipette etc.

Theory:

It is the lowest temp. at which the sample is completely miscible with equal vol. of
aniline. And the Mixed Aniline point: The minimum equilibrium soln. temp. of a
mixture of two volume of aniline, 1vol. of sample and 1vol. of n- heptane of
specific purity.Aniline point of a oil gives the indication of possible detoration of a
rubber sealing, packaging etc. in contact with oil. The aromatic hydrocarbon has a
tendency to dissolve certain type of rubber, so low aromatic content is desired for
the oil. Lighter the paraffin content, higher is the aniline point and cetane number
at the same time minimum is the knocking in the diesel fuel.

Apparatus:

 Automatic Anniline Point Apparatus

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 Heating and Cooling Bath: A suitable air bath, a nonvolatile, transparent

liquid bath, or an Infrared lamp provided with means for controlling the rate
of heating.

 Thermometer

 Pipette

 Glass stirrer

 Balance

 Safety Goggles and gloves

 Reagents: Deisel and Anniline

Procedure:

 Clean and dry the ‘U’ tube and arrange the apparatus desired.

 Now add 20ml. of distilled aniline and 20ml. of given sample in the ‘U’
tube, it will form two layers. Arrange the apparatus with stirrers in such way
that liquid in ‘U’ tube and the paraffin of the beaker are stirred
simultaneously.

 Switch on the heater to heat the paraffin at a controlled rate, so there is no

much difference in temp. of paraffin bath and ‘U’ tube.

 The minimum temp. at which two layers give a single phase is noted as
aniline point. Now stirring of ‘U’ tube mixture is stopped, and mixture is
allowed to cool.

 Temperature at which two layers are formed is also considered as aniline

point.
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 For mixed aniline point the above procedure is repeated by taking 10ml. of
sample, 10ml. of n-heptane and 20ml. of aniline.

Result:

Aniline point of the given sample = 73C

Conclusion

The aniline point of an oil is defined as the minimum temperature at which equal
volumes of aniline and lubricant oil are miscible, i.e. form a single phase upon
mixing..The value 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.The
aniline point serves as a reasonable proxy for aromaticity of oils consisting mostly
of saturated hydrocarbons (i.e. alkanes, paraffins) or unsaturated compounds
(mostly aromatics). Significant chemical functionalization of the oil (chlorination,
sulfonation, etc.) can interfere with the measurement, due to changes to the
solvency of the functionalized oil.

Penetration of the petroleum products

Theory:

This test method covers determination of the penetration of semi solid and solid
bituminous materials. The needles, containers and other conditions described in
this test method provide for the determinations of penetration up to 500.

Procedure:

The sample is melted and cooled under controlled conditions. The penetration is
measured with a Penetrometer by means of which a standard needle is applied to
the sample under specified conditions. The penetration test is usually used as a
measure of consistency.
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Apparatuses used:

Manual penetrometer.

46.5 grams plunger.

Weights, 50 grams and 100 grams.

Proximate Analysis of coal

 The proximate analysis of coal separates the products into four groups:

 Moisture

 volatile matter consisting of gases and vapors driven off during pyrolysis

 fixed carbon, the nonvolatile fraction of coal ash, the inorganic residue
remaining after combustion.

The proximate analysis of coal is presented as a group of test methods that has
been used widely as the basis for coal characterization in connection with coal
utilization. The methods for the determination of the total moisture in coal have
been placed into the following categories: thermal methods, a desiccator method,
distillation method, chemical methods, and electrical methods. The determination
of the volatile matter content of coal is an important determination because volatile
matter data are an integral part of coal classification systems and also form the
basis of evaluating coals for their suitability for combustion and carbonization.

Moisture content in coal

Free water may exist in the coal as adsorbed on the surface, condensed inside fine
capillary network and as bound to the coal molecule by chemisorptions and
hydrogen bonding. Moisture content is an important parameter in coal analysis. It
is needed for determining the calorific (heating) value and handling properties of a
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coal. The moisture value given for a proximate analysis is the moisture measured
as mass lost from a sample under specified conditions after heating in a moisture
oven to 104 to 110°C. This measured result is termed residual moisture. This is the
moisture value used for calculating other analytical results to a dry basis. It can be
used in conjunction with air-dried moisture to calculate on an as-received basis.

There are several sources of the water that occurs in coal and all coals are mined
with some water, such as: (1) adventitious moisture, which consists of groundwater
and other extraneous moisture and can be evaporated, (2) inherent moisture, which
occurs within the pore systems of the coal and is analyzed quantitatively, and (3)
adventitious moisture, which is removed by evaporation in air. Furthermore,
moisture in coal may also be classified into four possible forms within coal: (1)
surface moisture, which is water that is held on the surface of coal particles or
macerals, (2) hydroscopic moisture, which is water held by capillary action within
the micro-structure of the coal, (3) moisture which is produced by thermal
decomposition of the organic matrix of the coal and was part of the original
organic precursors, and (4) mineral moisture, which comprises part of the crystal
structure of hydrous silicates such as clay minerals.

Apparatus Required:
 Crucible

 Weighing Balance

 Oven

 Desiccator

Procedure
An empty weighing vessel is heated at 108±2 °C and weighed after cooling for 20
min. The air-dried material is crushed to pass 2.9 mm IS sieve. About 10 g of the
crushed material is then spread uniformly in the weighing vessel and weighed. The
uncovered vessel is heated in the drying oven at a temperature of 108±2 °C. until
there is no further loss in mass. This normally takes 1.5 to 3 h. The cover is
replaced and cooled in a desiccator for 20 min and then weighed.

Total moisture =X+Y*(1-X/100)

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Where,

X: percentage loss in mass of original in air-drying,

Y: percentage loss in mass of air dried sample on oven drying.

Calculations (M1)
Weight of petri dish (m1) = 23g

Weight of dish + sample before heating (m2) = 123g

Weight of sample (m3) = 100g

Weight of dish + sample after heating (m4) = 120g

Loss in weight (m5) = 3g

% moisture content = 3%

Ash Content in Coal

Ash yield is one of the most common parameters measured in coal. Ash yield is
measured to determine how much material remains (called ash residue) after a coal
is combusted. Ash yield is measured directly in an automated proximate analyzer
or ashing furnace. Results are presented in weight percent.

For this test, a coal sample is ground to a set size (-60 mesh, less than or equal to
250 micron particle size), weighed, and then combusted at temperatures between
500 and 750°C for 1 hour. The weight of the material that remains after
combustion is then compared to the original weight of the sample to measure the
percent ash yield. The ash yield or residue from a coal sample is largely composed
of the mineral matter in the coal, but does not equal the original mineral matter
content of the coal, because some of the minerals or mineral phases in the original
coal sample (e.g., sulfides and carbonates) are destroyed or converted to other
mineral compounds during combustion. Ash yield is an important parameter for
steam coals and for coals used in industrial furnaces. Increasing ash yield
corresponds to lower heating (calorific) value. Most steam coals used for
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electricity require less than 20 percent ash content (air-dried), and less than 10
percent ash is required in most utility contracts.

Apparatus Required:

 Silica Crucible

 Muffle furnace

 Tong

 Desiccators

 Weighing Balance

Procedure

In this test method, the coal sample is placed in a cold furnace and heated
gradually so the temperature reaches 450–500 ∘C (840–930 ∘F) in 1 h and 700–750
∘C (1290–1380 ∘F) at the end of the 2 h – the ISO method (ISO 1171)
recommends a final temperature of 815 ∘C (1500 ∘F). In both methods, the sample
is ignited at the appropriate final temperature to constant weight. Typically, the
experimental data should be reproducible within ±0.2% of the end result. There are
also other methods, predominantly thermal, which can be used for the analysis of
coal ash.

The important weights in this determination are those with the coal in the dish
before and after drying, the difference between them giving the weight of moisture
expelled. These must be determined, therefore, as accurately as possible and, to
enable this to be accomplished, the weight of the dish alone should be as small as
possible. Suitable petri dishes of thin glass and measuring 5 cm in diameter and 1
cm in height meet all the requirements of weight and area. If the coal under
investigation oxidizes appreciably at 100 ∘C (212 ∘F), it is often be necessary to
carry out the determination in an inert atmosphere either by passing a current of
oxygen-free nitrogen through the oven or by using an oven that can be evacuated.
In either case, it is an advantage to keep the free space in the oven down to a
minimum so as to render more effective the displacement action of the nitrogen or
the attainment of a suitable vacuum.

Calculations (M2)
Weight of petri dish (m1) = 23g
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Weight of dish + sample before heating (m2) = 120g

Weight of sample (m3) = 97g

Weight of dish + sample after heating (m4) = 100g

Loss in weight (m5) = 2g

% age ash content = 21%

Percentage of Volatile Matter

Volatile matter is one of the most common parameters measured in coal. It is part
of a standard proximate analysis. Volatile matter is essentially a measure of the
nonwater gases formed from a coal sample during heating. It is measured as the
weight percent of gas (emissions) from a coal sample that is released during
heating to 950 C° in an oxygen-free environment, except for moisture (which will
evaporate as water vapor), at a standardized temperature. Volatile matter is
measured directly in the automated proximate analyzer. Results are presented in
weight percent. Volatile matter is directly related to coal rank; as rank increases,
volatile matter content decreases. Volatile matter has the opposite trend of fixed
carbon with rank. As volatile matter is driven from the coal matrix with increasing
rank, the relative carbon percentage tends to increase. Both volatile matter and
fixed carbon are used to define coal rank in high-volatile, medium-volatile
bituminous, and higher-rank coals in the U.S. classification system.

Apparatus Required

 Silica Crucible

 Oven

 Muffle Furnace

 Pair of Tongs

 Desiccator

 Weighing Balance
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Procedure:
In the test method (ASTM D3175), one gram of coal is weighed and placed in a
pre-weighed platinum crucible (10–20 ml capacity, 25–35 mm in diameter, and
30–35 mm in height) with a close-fitting cover. The crucible is then suspended at a
specified height in the furnace chamber. The temperature of the region in the
furnace where the crucible is suspended must be maintained at 950±20 ∘C
(1740±36 ∘F). After the more rapid discharge of volatile matter, as evidenced by
the disappearance of the luminous flame, the cover of the crucible should be
tapped to ensure that the lid is still properly seated to guard against the admission
of air. After heating for exactly seven minutes, the crucible is removed from the
furnace and cooled. The crucible should be weighed as soon as it is cold. The
percentage loss of weight minus the percentage moisture equals the volatile matter.
The residue in the crucible is coke and it is often advantageous to indicate the
nature of the coke button obtained, since it provides a useful guide to the caking
properties of the coal. It is usually described under the following headings: color,
luster, swelling, fissuring, structure, both internal and surface, and hardness.

Calculations (M3)
Weight of Crucible (m1) = 23g

Weight of dish + sample before heating (m2) = 100g

Weight of sample (m3) = 77g

Weight of dish + sample after heating (m4) = 83g

Loss in weight (m5) = 17g

% age volatile content = 22%

Fixed Carbon in Coal

Fixed carbon is a measure of the amount of non-volatile carbon remaining in a coal

sample. It is a calculated value determined from other parameters measured in a
proximate analysis, rather than through direct measurement. Fixed carbon is the
calculated percentage of material that was lost during the testing for moisture,
volatile matter, and ash.
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Calculations

Fixed Carbon (%) = 100-M1-M2-M3

Specific Gravity of Petroleum products

Theory:
The specific gravity of an object is the ratio between the density of an object to a
reference liquid. The specific gravity has no units. If the specific gravity has a
value of greater than one, then the object sinks in water and if it is less than one,
then the object floats in water.
OBJECTIVE:
The objective of this experiment is to determine the specific gravity and API
gravity of different crude oils, liquid petroleum products, and mixtures of
petroleum and non-petroleum products by using a glass hydrometer. This
experiment will follow the standard method ASTM D 1298- 85, IP 160/96.
INTRODUCTION:
Density of crude oil is defined as the mass per volume. It is most often for oils in
units of gram / ml, and less often in units kg / m3. Density is temperature
dependent; it decreases with increase in temperature. All fresh crude oils and most
fuel oils have densities less than 1.0 gm/ml, but bitumen and certain fuel oils may
densities greater than 1.0 gm/ml. The density of crude oil changes with time as the
more volatile (and less dense) components are lost.
Two densities –related properties of oils are often used: specific gravity (Spgr.),
and American Petroleum Institute (API) gravity. Specific gravity or relative
density is the ratio, at a specified temperature, of the oil density to the density of
pure water.
Calculations:
The API gravity is calculated as:

API Gravity (o) = 141.5- 131.5/Specific gravity (60/60oF)

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Oils with low densities, and hence low specific gravities, have high API gravity.
The specific gravity of crude oil usually range from about 0.8(45.3o API ) for
lighter crude oils to over 1.0 (10o API) for heavy crude oils and bitumen. The price
of a crude oil is usually based on its API gravity, with high API gravity oil
commanding higher prices, because it can produce more quantity of the light
products in the refining processes, as well as low technical problems associated
with high API gravity which is related with low content of sulphur, asphaltenes,
metals, -------etc., in the crude.
Procedure:
 Clean and dry the Pycnometer. Tightly screw its cap. Take its mass (M1) to
the nearest of 0.1 g.
 Mark the cap and Pycnometer with a vertical line parallel to the axis of the
Pycnometer to ensure that the cap is screwed to the same mark each time.
 Unscrew the cap and place about 200 g of oven dried soil in the Pycnometer.
Screw the cap. Determine the mass (M2).
 Unscrew the cap and add sufficient amount of de-aired water to the
Pycnometer so as to cover the soil. Screw on the cap.
 Shake well the contents. Connect the Pycnometer to a vacuum pump to
remove the entrapped air, for about 20 minutes for fine-grained soils and
about 10 minutes for coarse-grained soils.
 Disconnect the vacuum pump. Fill the Pycnometer with water, about three-
fourths full. Reapply the vacuum for about 5min till air bubbles stop
appearing on the surface of the water.
 Fill the Pycnometer with water completely upto the mark. Dry it from
outside. Take its mass (M3).
 Record the temperature of contents.
 Empty the Pycnometer. Clean it and wipe it dry.
 Fill the Pycnometer with water only. Screw on the cap upto the mark. Wipe
it dry. Take its mass (M4).
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