PETROLEUM TESTING LABORATORY

DEPARTMENT OF CHEMICAL ENGINEERING

M.TECH. PETROLEUM REFINING AND PETROCHEMICALS

CONTENTS

Sl.No. Date Name of the Experiment Page No.

1 Flash and Fire point

2 Redwood Viscometer

3 Saybolt Viscometer

4 Engler Viscometer

5 Distillation Characteristics

6 API Gravity

7 Moisture content Determination

8 Softening Point

9 Smoke Point

10 Aniline Point

11 Cloud and Pour Point

12 Melting Point of Wax

13 Copper Strip Corrosion Test

14 Congealing Point of Wax

 FLASH POINT AND FIRE POINT

BY PENSKY MARTENS APPARATUS

AIM

To determine the flash point and fire point of fuel oils by using Pensky Martens apparatus
(closed type).

DEFINITION

FLASH POINT
The lowest temperature of the sample, corrected to a barometric pressure of 101.3 kPa 760
mm Hg , at which application of a test flame causes the vapour of the sample to ignite under
specified conditions of test.

FIRE POINT
The fire point, is defined as the temperature at which the vapour continues to burn after being
ignited.

SUMMARY OF METHOD

The sample is heated at a slow, constant rate with continual stirring. A small flame is directed
into the cup at regular intervals with simultaneous interruption of stirring. The flash point is
the lowest temperature at which application of the test flame causes the vapour above the
sample to ignite.

SIGNIFICANCE

• Flash point measures the response of the sample to heat and flame under controlled
laboratory conditions.
• It is only one of a number of properties which must be considered in assessing the
overall flammability hazard of a material.
• Flash point is used in shipping and safety regulations to define ‘flammable’ and
‘combustible’ materials.

APPARATUS

 Pensky Martens Closed Tester

  Thermometers (Two standard thermometers shall be used with the Pensky-Martens
tester)

TABULATION

S.No. SAMPLES FLASH POINT (ºC) FIRE POINT(ºC)

PREPARATION OF SAMPLE

Samples of asphalts or very viscous materials may be warmed until they are reasonable fluid
before they are tested. However, no sample should be heated more than is absolutely
necessary. It shall never be heated above a temperature of 17°C ( 30°F ) below its expected
flash point.

APPARATUS SPECIFICATIONS

A typical assembly of the apparatus, gas heated, is shown in Fig. The apparatus shall consist
of a test cup, cover, and stove conforming to the following requirements.

Cup - The cup shall be of brass, or other non-rusting metal of equivalent heat conductivity,
and shall conform to the dimensional requirements

Cover Proper - The cover shall be brass, and shall have a rim projecting downward almost
to the flange of the cup. The rim shall fit the outside of the cup with a clearance not
exceeding 0.36 mm 0.014 in on the diameter.

Shutter - The cover shall be equipped with a brass shutter approximately 2.4 mm ( 3/32 in )
thick operating on the plane of the upper surface of the cover. cover openings shall be exactly
open and the tip of the exposure tube shall be fully depressed.

Flame Exposure Device - The flame-exposure device shall have a tip with an opening 0.69
to 0.79 mm (0.027 to 0.031 in) in diameter. This tip shall be made preferably of stainless
steel, although it may be fabricated of other suitable metals

Pilot Flame - A pilot flame shall be provided for automatic relighting of the exposure flame.

Stirring Device - The cover shall be equipped with a stirring device mounted in the centre of
the cover and carrying two 2-bladed metal propellers.

Stove
Heat shall be supplied to the cup by means of a properly designed stove which is equivalent
to an air bath. The stove shall consist of an air-bath and a top plate on which the flange of the
cup rests.

Air Bath
The air bath shall have a cylindrical interior and shall conform to the dimensional
requirements in Fig.

Top Plate
The top plate shall be of metal, and shall be mounted with an air gap between it and the air
bath.

PROCEDURE

 The oil cup was cleaned using solvent.

 The cup was filled with fresh sample up to the mark.
 The cup was placed in the apparatus bath.
 The lid is placed on the cup and the thermometer was also inserted.
 The electrical heater was turned to 50% of input volts and oil is heated.
 After that spring handle was rotated at every degree rise from this point.
 The temperature was noted at which the flash occurs.
 The fire point was noted at which the fuel burnt continuously for 5 seconds.
 The experiment was repeated for different samples.

RESULT
Flash point and fire point of given samples are ________________ is _______ oC
 REDWOOD VISCOMETER

AIM

To determine the kinematic viscosity of the given sample of oil at various

temperatures and to study corresponding variation with respect to temperature.

APPARATUS REQUIRED

• Red wood viscometer with accessories

• Measuring flask

• Thermometer

• Stop watch

THEORY

• Red wood viscometer is based on the principle of laminar flow through the
capillary tube of standard dimension under falling head. The viscometer
consists of vertical cylinder with an orifice at the center of the base of inner
cylinder.

• The cylinder is surrounded by a water bath, which can maintain temperature of

the liquid to be tested at required temperature. The water bath is heated by
electric heater.

• Cylinder which is filled up to a fixed height with liquid whose viscosity is to

be determined is heated by water bath to the desired temperature.

• Then orifice is opened and the time required to pass the 50cc of oil is noted.
With this arrangement variation of viscosity with temperature can be studied.

FORMULA

• In this case of red wood viscometer, the kinematic viscosity (v) of liquid and
the time (t) required to pass 50cc of liquid are correlated by expression.

ν =0.0026 – 1.175/t

Where,

• ν = Kinematic viscosity
 • t =time in seconds to collect 50cc of oil.

OBSERVATION

Sl.No. Temperature (0C) Time taken to collect 50cc of oil Kinematic viscosity
(sec) (centistokes)
SIGNIFICANCE

• Pump design can be done with the help of viscosity.

• Pump operation of the engine depends on the proper viscosity of the liquid
fuel.

• It’s very important to know about the fluid flow through various objects.

• Conveying of fluid can be done effect by means of viscosity data.

PROCEDURE

• The instrument was leveled with the help of the circular bubble and by
leveling foot screws.

The water bath was filled with water.

The orifice is closed with the ball valve and the cylinder is filled up to index
mark with oil.

The steady state temperature of oil was recorded.

The procedure is repeated for different by heating oil with water bath.
RESULT

The kinematic viscosity for the given sample was determined and the graph was
plotted and it was observed that the kinematic viscosity of the given sample decreases
with increases in temperature.

SAYBOLT VISCOMETER
 SAYBOLT VISCOMETER

AIM

To determine the viscosity of the given petroleum products and to study the
variation of viscosity with respect to temperature.

APPARATUS REQUIRED
∗ Saybolt viscometer apparatus
∗ Thermometer (0 – 100 deg)
∗ Sample
∗ Stop watch
∗ Beaker (100 ml capacity)

THEORY
Viscometers are used to define the viscous properties of a fluid at ambient or defined
temperatures. They are commonly available in the form of a calibrated capillary tube through
which a liquid is allowed to pass at a controlled temperature in a specified time period. Other
methods include rotational viscometry and falling ball tests. Viscometers can have a few
different technologies by which they operate.

For rotational viscometry, torque is required to rotate a spindle at constant speed

while immersed into the sample fluid. The torque is proportional to the viscous drag on the
immersed spindle, and thus to the viscosity of the fluid. For falling ball technology, the
viscosity is proportional to the time required for a ball to fall through the test liquid contained
in a precise an temperature controlled glass tube. Capillary viscometers measure the flow rate
of a fixed volume of fluid through a small orifice at a controlled temperature.

The time it takes for a specific volume of fluid to pass through the orifice is
proportional to the fluid viscosity. However, it also depends on the density of the fluid since
the denser the fluid, the faster it will flow through the orifice. The property being measured is
then the kinematic viscosity and not the dynamic viscosity.

TYPES OF VISCOMETERS
• Reverse flow viscometers
• Small volume viscometers
• Viscometers
• Vacuum viscometers
• Cylinder viscometers
• Hydra motion viscometers

OBSERVATION

S.No. Temperature (0C) Time (seconds) Kinematic viscosity (centistokes)

FORMULA
Kinematic viscosity, ν = At-B/t
Where, A=0.00226, B=1.95
A and B are constants.

SAFETY PRECAUTIONS
• Do not connect bath to a power supply unless the bath is filled with oil.
• Do not leave unit unattended, especially when operating at high bath
temperatures.
• This could create a potential fire hazard.

SIGNIFICANCE
• It is used to find the viscosity of the fluid.
• Pump design can be done with the help of viscosity.
• Pump operation of one engine depends on the proper viscosity of fuels.
• Conveying of fluids can be done with the help of viscosity data.
• It is very important to know about the fluid flow through various objects.

EXPERIMENTAL PROCEDURE
• The viscometer was turned on after making sure that the bath was filled with oil.
• The bath was heated by means of water heater.
• The power switch was turned on. The bath temperature was maintained at various
temperatures.
• The bath was allowed to reach a steady temperature.
 • The cork stopper is used to block off the outlet of one of the Saybolt viscometer
tubes.
• A measured quantity (+60 ml) of the sample was poured into the tube.
• The sample temperature was allowed to equilibrate with that of the bath (about 25
minutes).
• Simultaneously the Saybolt tube was uncorked (using the pull chain) and the
stopwatch was started.
• When the oil has reached the 60 ml mark, the stopwatch was stopped. The time
was recorded. The experiment was repeated for various temperatures.

RESULT
Thus the kinematic viscosity for given sample was determined for different temperatures
and tabulated. The graph was plotted and it was found that the kinematic viscosity decreases
with increase in temperature.

ENGLER VISCOMETER
DETERMINATION OF KINEMATIC VISCOSITY BY ENGLER VISCOMETER
AIM

To determine the kinematic viscosity of the given fluid using Engler viscometer.

APPARATUS REQUIRED

• Engler viscometer

• Timing device

• Thermometer

• Sample

THEORY

Specific viscosity of a substance in the Engler scale is the time required in seconds for
the flow of 100cc of the sample divided by the time taken for the flow of equal volume of
water. This viscometer allows direct comparison of viscosities of various samples without
lead to calculate their actual viscosities.

Viscosity

. Viscosity is the ratio between the shear stress and the velocity gradient. In other
words, viscosity is the resistance offered by the fluid. The unit of viscosity is centipoises. In
SI, kg/ms.

Newton’s law of viscosity

The shear stress is the product of absolute viscosity and velocity gradient.

τ = µ (dv/dx)

Kinematic viscosity
 It is defined as the ratio between the absolute viscosity and density, denoted by ν.

ν=µ/ρ

The unit of kinematic viscosity is centistokes.

Range of Engler viscometer

Temperature measurement range 0-100oC

Viscosity range of fluids 28.8 – 35.2 centistokes

OBSERVATION

TIME (sec) KINEMATIC

VISCOSITY
S.No TEMPERATURE

SAMPLE WATER t (sec) (centistokes)

(OC )
SIGNIFICANCE

• In the determination of specific viscosity of tars and the fluid properties.

• In the determination of lubricating properties of fuel oils.

FORMULA

1) ν = At – (B/t)

where ν = kinematic viscosity (centistokes)

A, B = constants

A = 0.076, B = 0.04

2) t = (t1-t2)/60

where t = efflux time in seconds

t1 = time taken for collecting sample (sec)

t2 = time taken for collecting water (sec)

EXPERIMENTAL SETUP

It consists of a water bath having oil cup with lid. The water stirring device is
mounted on a stand. Thermometer is dipped in water bath with help of clamp. The lid of the
oil cup has a thermometer holder. The bath is fitted with water heater. It can be operated on
200 volt AC mains.

PROCEDURE

• The given sample was filled in the cup of the Engler viscometer up to the level
marked.
 • The lid was closed to prevent vaporisation of sample.

• The heater was switched on and the water temperature was noted.

• The water was stirred well to promote uniform heat distribution around the oil.

• When the temperature reaches specific value, heating was stopped and the stalk was
removed.

• The time taken for flow of 100ml sample was noted.

• The orifice is closed again and the sample was refilled into the cup.

• The procedure was repeated for different temperatures and the readings were
tabulated.

• The above procedure was also repeated by filling the cup with water.

RESULT

The viscosity of the given sample was determined at various temperatures and graph
was plotted. It is found that kinematic viscosity decreases with increase in temperature.
 DISTILLATION CHARACTERISTICS

SCOPE
To determine the distillation characteristics (boiling range) of the given sample using
the distillation apparatus.

DISTILLATION
This method of test covers the distillation of motor gasoline, aviation gasoline, aviation
turbine fuels, special boiling point spirits, naphtha, white spirit, kerosene, gas oils, distillate
fuel oils and similar petroleum products. A 100 ml sample is distilled under prescribed
conditions which are appropriate to its nature. Systematic observations of thermometer
readings and volumes of condensate are made, and from the data, the results of the test are
calculated and reported.
The distillation (volatility) characteristics of hydrocarbons have an important effect on their
safety and performance, especially in the case of fuels and solvents. The boiling range gives
information on the composition, the properties, and the behavior of the fuel during storage
and use. Volatility is the major determinant of the tendency of a hydrocarbon mixture to
produce potentially explosive vapors.
The distillation characteristics are critically important for both automotive and aviation
gasoline, affecting starting, warm-up, and tendency to vapor lock at high operating
temperature or at high altitude, or both. The presence of high boiling point components in
these and other fuels can significantly affect the degree of formation of solid combustion
deposits.
Distillation limits are often included in petroleum product specifications, in commercial
contract agreements, process refinery/control applications, and for compliance to regulatory
rules.
This test method can be applied to contaminated products or hydrocarbon mixtures. This is
valuable for fast product quality screening, refining process monitoring, fuel adulteration
control, or other purposes including use as a portable apparatus for field testing.

SIGNIFICANCE
 Distillation (volatility) characteristics of petroleum products are indicative of
performance in their intended applications.
 Petroleum product specifications generally include distillation limits to ensure
products of suitable volatility performance.
 The empirical results obtained by use of this distillation method have been found
to correlate with automotive equipment performance factors and with other
characteristics of petroleum products related to volatility.
 For motor spirit the 10% distillation value gives an indication of the engine start
conditions, also the final boiling point.
 OBSERVATION

S.No Volume of Distillate collected Temperature ºC

(ml)
TERMINOLOGY

Initial Boiling Point

The thermometer reading which is observed at the instant that the first drop of condensate
falls from the lower end of the condenser tube,

End-Point or Final Boiling Point

The maximum thermometer reading obtained during the test. This usually occurs after the
evaporation of all liquid from the bottom of the flask. The term ‘maximum temperature’ is a
frequently used synonym.

Dry Point
The thermometer reading observed at the instant the last drop of liquid evaporates from the
lowest point in the flask. Any drops or film of liquid on the side of the flask or on the
thermometer are disregarded.

Decomposition Point
The thermometer reading which coincides with the first indication of thermal decomposition
of the liquid in the flask.

Percent Recovered
The volume in ml of condensate observed in the receiving graduate, in connection with a
simultaneous thermometer reading.

Percent Recovery
The maximum percent that is recovered.

Percent Total Recovery

The combined percent recovery and residue in the flask.

Percent Loss
100 minus the percent total recovery.
Percent Residue
The percent total recovery minus the percent recovery, or the volume of residue in milliliters
if measured directly.
Percent Evaporated
The sum of the percent recovered and the percent loss.
PROCEDURE

 The given flask is to be thoroughly cleaned using solvent and dried.

 The given test sample is then taken inside the flask and the cork with appropriate
thermometer is placed on the neck of the flask.
 The flask is placed on the asbestos board and fixed to the metal condensers with a
cork. The asbestos board is raised of lowered till the flask is properly supported.
 The 100cc measuring cylinder is placed below the condenser outlet. The heater is then
switched on and the temperature variation is noted.
 The temperature at which the first drop of distillate is collected in the measuring
cylinder is noted and reported as the initial boiling point.
 Heat is controlled, so that the distillation process is at a uniform state.
 Middle boiling point is the temperature at which 50% of oil distills off.

RESULT
The Distillation characteristics are studied for the given samples and the values are noted as
follows:
1. Initial boiling point = º C
2. Middle boiling point = º C
3. Percentage of recovery =
4. Percentage of non-volatile residue =
5. Film boiling point = º C
API GRAVITY - DIAGRAM
 DETERMINATION OF API GRAVITY OF CRUDE PETROLEUM AND LIQUID
PETROLEUM PRODUCTS BY HYDROMETER METHOD AND SPECIFIC
GRAVITY BOTTLE METHOD

AIM

To determine the API gravity of crude petroleum and liquid petroleum products by
hydrometer method and specific gravity bottle method.

THEORY

This method covers the laboratory determination, using a glass hydrometer, of the
density, relative density, or API gravity of crude petroleum, petroleum products, or mixtures
of petroleum and non-petroleum products normally handled as liquids and having a Reid
vapour pressure of 1.8 bar (179 KPa) or less. The values are measured on a hydrometer at
convenient temperatures, readings of density being reduced to 15 oC, and that of specific
gravity and API gravity to 15.6 oC, by means of international standard tables.

CLASSIFICATIONS OR GRADES

Crude oil is classified as light, medium or heavy, according to its measured API gravity.

• Light crude oil is defined as having API gravity higher than 31.1 °API.
• Medium oil is defined as having API gravity between 22.3 °API and 31.1 °API.
• Heavy oil is defined as having API gravity below 22.3 °API.

SIGNIFICANCE

Accurate determination of density, relative density, or API gravity of petroleum and

its products is necessary for the conversion of measured volumes to volumes at standard
temperature of 15°C.

FORMULA

API Gravity

A special function of specific gravity at 15.6/15.6 oC is represented by:

API gravity, degrees = [141.5 /Specific gravity at 15.6/15.6 oC] - 131.5

APPARATUS REQUIRED

• Hydrometer
• Hydrometer cylinders
• Specific gravity bottle
 OBSERVATIONS

SPECIFIC GRAVITY

Sl.No SAMPLES
At room temperature At room temperature
using Hydrometer using Specific gravity
bottle method

SPECIFIC GRAVITY BOTTLE METHOD

Weight of the empty specific gravity bottle =

Weight of the specific gravity bottle with sample 1 =

Weight of the specific gravity bottle with sample 2 =

Weight of the specific gravity bottle with sample 3 =

Weight of the specific gravity bottle with sample 4 =

PROCEDURE

Hydrometer method

• The samples were transferred to hydrometer cylinders without any splashing to avoid
air bubbles.
• The cylinders containing samples were placed in vertical position in a location free
from air currents.
• The hydrometer was gently lowered into the sample in cylinders such that the
hydrometer should not touch the walls of the cylinder.
• The hydrometer was allowed to float and when it comes to rest, the specific gravity
indicated by the hydrometer for different samples at room temperature were noted.
• From the specific gravity values the API gravity for the given samples were
calculated.
Specific gravity bottle method

• The samples were taken in each specific gravity bottle.

• The specific gravity bottle with the samples and the weight of the empty specific
gravity bottle were measured.
• The readings were tabulated and the specific gravity for different samples was
calculated. From the specific gravity values the API gravity for the given samples
were calculated.

RESULT

The API gravity of the given samples using hydrometer and specific gravity bottles
were calculated and tabulated as follows

API gravity

Sl.No. Samples
Hydrometer method Specific gravity bottle
method
DETERMINATION OF MOISTURE CONTENT BY DEAN AND STARK
METHOD

SCOPE

To estimate the moisture content of the given liquid fuel using Dean and Stark Apparatus.

EXPERIMENTAL SETUP

The Dean-Stark apparatus or Dean-Stark receiver or distilling trap is a piece of

laboratory glassware used in synthetic chemistry to collect water (or occasionally other
liquid) from a reactor. It is used in combination with a reflux condenser and a batch reactor
for continuous removal of the water that is produced during a chemical reaction performed at
reflux temperature. It was invented by E. W. Dean and D. D. Stark in 1920 for determination
of the water content in petroleum. The Dean-Stark trap (1920) changed the distillation
procedure from a simple distillation to a multiple distillation by a change in design where by
a refluxing condenser was introduced .This change resulted in a smaller boiling flask and
required less distilling liquid. It renewed the interest in the distillation procedure, for it
enabled the last traces of water.

DEAN AND STARK APPARATUS

Two types of Dean-Stark traps exist – one for use with solvents with a density less than water
and one for use with solvents with a density greater than water.

The Dean-Stark apparatus in the laboratory typically consists of vertical cylindrical piece of
glass (the trap, in figure), often with a volumetric graduation on its full length and a precision
tap on the bottom very much like a burette. The top of the cylinder is fit with the bottom of
the reflux condenser. Protruding from the top the cylinder has a side-arm sloping toward the
reaction flask. At the end the side-arm makes a sharp turn so that the end of the side arm is
vertical as well. This end connects with the reactor.

SIGNIFICANCE

 This piece of equipment is usually used in azeotropic distillations. A common

example is the removal of water generated during a reaction in boiling toluene.
 The Dean-Stark method is commonly used to measure moisture content of items such
as bread in the food industry.
 This equipment can be used in cases other than simple removal of water. One
example is the esterification of butanol with acetic acid catalyzed by sulfuric acid
 The Dean and Stark procedure can be used to measure the water content of a diverse
range of samples, and has been extensively used in industrial laboratories to measure
water in petroleum oils.
PRINCIPLE

During the reaction in , vapors containing the reaction solvent and the component to be
removed travel out of reaction flask up into the condenser ,and then drip into the distilling
trap .Here, immiscible liquids separate into layers. When the top (less dense) layer reaches
the level of the side-arm it can flow back to the reactor, while the bottom layer remains in the
trap. The trap is at full capacity when the lower level reaches the level of the side-arm--
beyond this point, the lower layer would start to flow back into the reactor as well. It is
therefore important to syphon or drain the lower layer from the Dean-Stark apparatus as
much as needed.

More rarely encountered is the model for solvents with a density greater than water. This type
has a tube at the bottom of the side-arm to allow the organic solvent at the bottom to flow
back into the reaction vessel. The water generated during the reaction floats on top of the
organic phase. An azeotropic mixture of toluene and water distills out of the reaction, but
only the toluene (density=0.865 g/ml) returns, since it floats on top of the water
(density=0.998 g/cm3), which collects in the trap. This equipment can be used in cases other
than simple removal of water. One example is the esterification of butanol with acetic acid
catalyzed by sulfuric acid. The vapor contains 63% ester, 24% water and 8% alcohol at reflux
temperature and the organic layer in the trap contains 86% ester, 11% alcohol and 3% water
which is reintroduced. The water layer is 97% pure. Another example is the esterfication of
benzoic acid and n-butanol where the ester product is trapped and the butanol, immiscible
with the ester flows back into the reactor. Removing water in the course of these
esterfications shifts the chemical equilibrium in favour of ester formation.

PROCEDURE

 A known volume of the fuel sample is to be placed in a flask with equal volume of
organic solvent such as xylene of toluene.
 The organic solvent is chosen such that it is insoluble in water. It should have a higher
boiling point than water and it should be safe to use.
 The flask containing the sample with the organic solvent is then attached to a condenser
by a side arm and the mixture is heated up.
 The water in the sample gets evaporated and moves into the condenser where it is cooled
and converted back into liquid water.
 The water trickles into the graduated tube. The distillation is then stopped and the water
present in the liquid fuel is measured.

RESULT

The amount of moisture content present in the sample was found using the Dean and Stark
apparatus to be
 SOFTENING POINT

AIM

To determine the softening point of the given sample bitumen using ball and ring
apparatus.

APPARATUS REQUIRED

 Ring and ball apparatus

 Steel balls
 Brass rings
 Thermometer
 Stirrer
 Water bath

SIGNIFICANCE

 To find the consistency of bitumen

 It is regarded by same indication of viscosity
 It is used in the designation of hard as oxidized bitumen.

THEORY

 The temperature at which the substance attains a particular degree of softness under
specified condition of test is called softening point.
 Bitumen is specified by softening point. Bitumen being amorphous does not melt
sharply but gradually becomes softer and less viscous as the temperature rises.
 For this reason, the determination of the softening point must be made by fixed
arbitrary and closely defined method.
 The softening point of bitumen is rounded out by the ball and ring test.

APPLICATION

 Used in annealing of bitumen.

 Processing of plastics.
 Determining the quality of bitumen.
PROCEDURE

 A beaker is taken and filled with ¾ of it with water.

 The sample is placed in the ring and the steel ball is kept over the sample at the
middle of the ring.
 The whole ring and ball is immersed into the beaker which is filled with water.
 The water in the beaker is heated by electrical coil.
 A thermometer is inserted to note the temperature.
 As the temperature increase, the sample gets softens and the steel ball over the sample
gets immersed and finally drops out.
 The temperature at which the ball falls down from the ring is noted as softening point
of the sample.
 The ring is washed and replaced with another sample and the process is repeated.

RESULT

 The softening point of given first sample =

  The softening point of given second sample =

FLAME HEIGHT

A-Too high

B- Correct

C-Too low
 SMOKE POINT

AIM

This method is intended for the determination of smoke point of kerosene and other
volatile liquid fuels including gas turbine (jet) fuels.

DEFINITION

The maximum flame height in millimetres at which kerosene or other volatile liquid
fuels including gas turbine (jet) fuels will burn without smoking, when determined in the
apparatus and under specified conditions.

OUTLINE OF THE METHOD

The sample is burned in a standard lamp in which it is possible to adjust the flame
height against a background of a graduated millimetre scale. The smoke point is measured by
raising the wick until a smoky flame is produced and then lowering to the point where the
smoky tail just disappears. This flame height, measured to the nearest millimetres, is the
smoke point of the sample

REQUIREMENTS:

 Smoke point apparatus

 Fuel samples

 Wick

Smoke Point Lamp - Constructed according to the specification given. The lamp consists of
an oil container provided with a wick tube and air vent, a gallery fitted with a wick guide and
provided with air inlets, a lamp body, and a chimney provided with a 50-mm scale specified

Oil Container - This shall conform to the following dimensions (mm):

Body Oil Container:

Internal diameter 21.25 ± 0.25
External diameter Sliding fit in holder
Length, without cap 109-00 ± 0.05
Thread on cap 9’5 mm dia screwed 1.0 mm pitch

Wick Tube:
Internal diameter 4’7 ± 0.05
External diameter Close fit in wick guide
Length 82.00 ± 0.05
 OBSERVATION

S. No. Sample(ml) Smoke Point(mm)

Air Vent:
Internal diameter 3.50 ± 0’05
Length 90.00 ± 0.05

Lamp - This shall conform to the following dimensions in mm:

Internal diameter of socket of oil container 23.80 ± 0.05
Internal diameter of wick guide 6.00 ± 0.02
Diameter of each of 20 air inlets 2.90 ± 0.05
x: External diameter of gallery 35.00 ± 0.05
Diameter of each of 20 air inlets in the gallery 3.50 ± 0.0.5
Internal diameter of lamp body 81.0 ± 1.0
Internal depth of lamp body 81.0 ± 1.0
Internal diameter of chimney 40.0 ± 1.0
Height, top of chimney to centre of lamp body 130.0 ± 1.0

Other Requirements - The lamp shall also comply with the following requirements:

a)The top of the wick guide shall be exactly level with the zero mark on the scale;
b) The scale shall be marked in white lines on black glass on each side of a white or black
strip, 2mm in width. It shall have a range of 50 mm, graduated in one millimetre, figured at
each 10mm, and with longer lines at each 5 mm;
c) A device for raising or lowering the flame shall also be provided.
The total distance of travel shall be not less than 10 mm, and the movement shall be smooth
and regular. Further, with the oil container in the lowest position and the .wick projecting 6
mm above the top of the oil container, the top of the wick shall not project above the wick
guide (zero on the scale );
d) The glass of the door shall be curved to prevent the formation of multiple images; and
e) The joint between the base of the oil container and its body shall be oil-tight.

Wick - Woven solid circular wick of cotton yarn and complying with the following
requirements shall be used:

Number of Threads
Casing 17 ends
Filling 9 ends
Picks 6 per cm

PRECAUTIONS

• The test shall normally be carried out at a room temperature of not less than 15°C; it
is recommended that the room temperature and the barometric pressure be recorded.
• Place the lamp in a vertical position completely protected from draughts.

PROCEDURE

• 20 ml of the previously filtered sample is introduced in the clean, dry oil container.
• A piece of wick is extracted, not less than 12’5 cm in length, with a suitable volatile
solvent and it is dried for half an hour at 100 to 110°C.
• The wick is soaked in the sample under test and is placed in the wick holder, carefully
easing out any twists arising from this operation. It is advisable to re-soak the burning
end of the wick in the sample.
• The wick holder is placed in the container and ensured that the air inlet is free from
oil. The wick is cut horizontally and trimmed to free the frayed ends so that 6 mm of
wick projects from the container.
• The oil container is maintained at a temperature of 20 to 25°C for 10 minutes. The
lamp is inserted and the wick is lighted.
• The wick is adjusted so that the flame is about 1 cm high and allows the lamp to burn
for 5 minutes. The wick is raised until a smoky tail appears, then lowered slowly
through the following stages of flame appearances:
a) A long tip, smoke slightly visible, erratic and jumpy flame.

b) An elongated pointed tip with the sides of the tip appearing concave upward.

c) The pointed tip just disappears leaving a very slightly blunted flame Jagged, erratic,
luminous flames are sometimes observed near the true flame tip. These are to be
disregarded.

d) The height flame is estimated to the nearest millimetre.

• The smoke point is recorded as observed. To eliminate errors due to parallax, the eye
of the observer should be slightly to one side of the centre line, so that a reflected
image of the flames seen on the scale on one side of the central vertical white line,
and the flame itself is seen against the other side of the scale. A sighting device may
also be used to eliminate parallax and to facilitate reading the flame height.
• The reading for both observations should be identical.
SIGNIFICANCE

• This is an important test for illumination oils for their ability to burn without
producing smoke.
• It is used in the assessment of burning quality of aviation fuel. Higher the smoke point
better is its domestic use.
• To find aromatic content of the kerosene.
• This test method provides an indication of the relative smoke producing properties of
kerosene’s and aviation turbine fuels in a diffusion flame. The smoke point is related
to the hydrocarbon type composition of such fuels.
• Generally the more aromatic the fuel the smokier the flame. A high smoke point
indicates a fuel of low smoke producing tendency.
• The smoke point (and Illuminometer number with which it can be correlated) is
quantitatively related to the potential radiant heat transfer from the combustion
products of the fuel. Because radiant heat transfer exerts a strong influence on the
metal temperature of combustor liners and other hot section parts of gas turbines, the
smoke point provides a basis for correlation of fuel characteristics with the life of
these components.

RESULT

S. No. Sample(ml) Smoke Point(mm)

Thus the smoke point experiment was performed and is tabulated below:
ANILINE POINT
AIM

To determine the aniline point of the given sample.

APPARATUS

• The tube approximately 25mm in diameter and 150mm in length made of heat-
resistant glass.

• A Jacket-approximately 37 to 42mm in diameter and 175mm in length made of heat-

resistant glass.

• A Stirrer-manually operated, approximately 2mm in diameter soft iron wire.

THEORY

Aniline point

Aniline is a poor solvent for aliphatic hydrocarbons and excellent one for aromatics.
This property is used in the aniline point test. Aniline point of oil is the lowest temperature at
which the oil is completely miscible with an equal volume of aniline.

Equal volumes of the sample and aniline (5 ml each) are heated or cooled with
stirring in a jacketed test tube and temperature at which complete miscibility occurs is noted.

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

Diesel index

Diesel index is an indication of the ignition quality of a diesel fuel. This is determined
by calculation from the specific gravity and the aniline point of the sample. Although it is of
the same order as the cetane number, it may differ widely from the cetane number. Higher the
diesel index better is the ignition quality of the diesel fuel. It is normally used as a guide to
ignition quality of the diesel fuel in the absence of test engine for the direct measurement of
cetane number.

The diesel index is calculated as follows:

(a) Diesel index = (Aniline point,ºF ׺API)/100

(b) Diesel index = (Aniline gravity constant)/100
(c) Diesel index = (Cetane number −10)/0.72

Cetane number
 Cetane number is related to the ignition delay of a fuel in a diesel engine, i.e. how
rapidly combustion begins after injection of the fuel into the combustion chamber.

The shorter the ignition delay period, higher is the cetane number of the fuel

Cetane number is the index of the ignition quality of a fuel. High cetane number
fuels will facilitate easy starting of compression ignition engines, particularly in cold
weathers, and faster warm up. These also result in increased engine efficiency and power
output, reduced exhaust smoke and odour and combustion noise. In the absence of test
engine, the diesel index or the calculated cetane index will give an approximate idea of the
ignition quality of the fuel.

Cetane number= 0.72×Diesel index + 10

PROCEDURE

• The apparatus was dried and cleaned.

• 10ml of aniline and 10ml of the sample were dried and pipetted into the test tube
fitted with stirrer and thermometer.

• The thermometer in the test tube was centered to make the immersion mark at the
liquid level; it is assured that the thermometer bulb does not touch the side of the tube.

• In the case of not mixing of aniline-sample at normal temperature, heat is applied

directly to the jacket tube so that the temperature raised at a rate of 1-3ºC/min till
complete miscibility was obtained.

• Stirring is continued and the mixture is allowed to cool at a rate of 0.5 to 1ºC/min.

• Cooling is continued to a temperature of 1 to 2ºC below the first appearance of

turbidity.

• The temperature at which the mixture suddenly became cloudy throughout is recorded
as the aniline point.

RESULT

Results for the aniline point experiment were found to be

• Aniline point =

• Diesel index =

• Cetane number =
CLOUD AND POUR POINT EXPERIMENTAL SETUP
 CLOUD AND POUR POINT DETERMINATION

AIM

To determine the Cloud point and pour point of the given sample.

REQUIREMENTS

Cloud and pour point apparatus, Thermometer, Ice crystals.

DEFINITIONS

The cloud point of a fluid is the temperature at which dissolved solids are no longer
completely soluble, precipitating as a second phase giving the fluid a cloudy appearance. This
term is relevant to several applications with different consequences.

Also, the pour point can be defined as the lowest temperature expressed in multiples of 3ºC
at which the oil is observed to flow when cooled and examined under prescribed conditions.

THEORY

Cloud point and pour point are indicators of the lowest temperature of utility for petroleum
products. Cloud Point gives a rough idea of temperature above which the oil can be safely
handled without any fear of congealing or filter clogging. The sample is periodically
examined while it is being cooled in the cloud and pour point apparatus. The highest
temperature at which haziness is observed (cloud point), or the lowest temperature at which
the oil ceased to flow is observed (pour point), is reported as the test result.

The cold filter plugging point test is used to determine the extent to which diesel fuel or gas
oil will flow, even though the temperature is below that at which wax crystals normally
appear, i.e. cloud point.
Pour point is a well established test to estimate the temperature at which a sample of oil
becomes sufficiently solid to prevent its movement by pumping. The pour point indicates the
waxy nature of the oils.

SAMPLES SHOWING CLOUD AND POUR POINT

PROCEDURE

Measuring cloud point of petroleum product:

The test oil is required to be transparent in layers 40mm in thickness (in accordance
with ASTM D2500). The crystals of the sample typically first form at the lower
circumferential wall with the appearance of a whitish or milky cloud. The cloud point is the
temperature at which these crystals first appear.
The test sample is first poured into a test jar to a level approximately half full. A cork
carrying the test thermometer is used to close the jar. The thermometer bulb is positioned to
rest at the bottom of the jar. The entire test subject is then placed in a constant temperature
cooling bath on top of a gasket to prevent excessive cooling.
At every 1°C, the sample is taken out and inspected for cloud then quickly replaced.
Successively lower temperature cooling baths may be used depending on the cloud point.
Lower temperature cooling bath must have temperature stability not less than 1.5 K for this
test.
Measuring pour point of petroleum product:

Two pour points can be derived which can give an approximate temperature window
depending on its thermal history. Within this temperature range, the sample may appear
liquid or solid. This peculiarity happens because sample crystals form more readily when it
has been heated within the past 24hrs and contributes to the lower pour point.
The upper pour point is measured by pouring the test sample directly into a test jar. The
sample is then cooled and then inspected for pour point as per the usual pour point method.
The lower pour point is measured by first pouring the sample into a stainless steel pressure
vessel. The vessel is then screwed tight and heated to above 100 oC in an oil bath. After a
specified time, the vessel is removed and cooled for a short while. The sample is then poured
into a test jar and immediately closed with a cork carrying the thermometer. The sample is
then cooled and then inspected for pour point as per the usual pour point method
RESULT

The pour point of the given sample was found to be ---------0C.

The cloud point of the given sample was found to be ---------0C

MELTING POINT DETERMINATION

AIM

To determine the melting point of given sample. And also its solidification point.

APPARATUS REQUIRED

 Thermometer

 Test tube

 Hot plate

 Burette stand

DEFINITION
When a solid substance is heated, typically it will melt; that is to say, at some
temperature the solid will begin to liquefy and by some slightly higher temperature all of the
solid will have become liquid. The melting point (actually melting point range) of a
compound is then defined as the temperature at which an observer can first see liquid forming
from the solid to the temperature where the last particle of solid has become liquid.

PURPOSE
 There are several purposes for doing this experiment. The first is to learn how to
determine the melting range of a solid substance accurately. When a solid substance is
prepared its melting point is usually determined to aid in its identification and to get
some idea of its purity.

 The second is to observe the effect of the purity of a substance on its melting
behavior. Pure substances usually have melting point ranges of a degree or two;
impure substances (which are mixtures of two or more substances) often have wider
ranges.

 The third is to use a physical constant of an unknown substance – its melting point –
to identify it from among several possibilities.

PROCEDURE
  Melting points are usually determined by placing one or two milligrams of the
material is to be tested into a melting point capillary, and heating the capillary and a
thermometer together, and observing over what temperature range the material melts.
The melting point capillary is a thin-walled glass tube, about 100 mm in length and
not more than 2 mm in outside diameter, sealed at one end.

 The bulb end of the thermometer is inserted, along with the attached capillary tube.
The capillary tube and the thermometer are clamped to the stand.

 The accurate melting point is achieved by heating the sample at a rate of 1 to 2

degrees per minute.

 If you have no idea what the melting point of your sample is, you have two choices at
this point. (1) You could start at room temperature and warm at the recommended rate
until the solid melts. This could take more than an hour. (2) You could start at room
temperature and warm at about 10 degrees a minute and obtain an approximate
melting point.

 Then, after the apparatus has cooled below the sample's melting point, replace the
sample (and capillary) with a new one, and heat slowly until the sample has melted,
thus getting an accurate melting point.

 The test tube is kept in air bath and the temperature is noted for every 30 seconds until
it gets completely solidified.

SIGNIFICANCE

It is used for compound identification and estimation of purity

MELTING POINT RANGE OF DIFFERENT COMPOUNDS

RESULT

Thus the melting point range of sample was determined from the graph. It is found to
be

COPPER STRIP CORROSION TEST – TEST BOMB

 COPPER STRIP CORROSION TEST

AIM

To detect the corrosiveness of the given sample using copper strip corrosion test.
PRINCIPLE

The method covers the detection of corrosiveness to copper of aviation gasoline from
tractor fuel, solvent, kerosene, diesel, fuel oil, lube oil, certain other petroleum products.

A polished copper strip is immersed in a given quantity of sample and heated at a

temperature and for a time characteristics of the material being tested. At the end of this
period, the copper strip is removed, washed and compared with copper strip corrosion
standards. It is particularly important that all types of feed sample which should pass a
tarnished strip classification. We collected clean glass bottles, plastic bottles or other suitable
containers that will not affect the corrosiveness properties of the sample.

REQUIREMENTS

• Copper strip corrosion test bomb

• Constant temperature water bath

• Polishing ice

• Glass test tube

• Polishing paper

SIGNIFICANCE AND USE

This test method is suitable for setting specifications, for use as an internal quality
control tool, and for use in development or research work on industrial aromatic
hydrocarbons and related materials. It also gives an indication of the presence of certain
corrosive substances which may corrode equipment, such as acidic compounds or sulfur
compounds.
PROCEDURE

• The test is to be operated at 50oC constant temperature.

• The bath is set at the desired working temperature and waits for 20 minutes of
time after the start.

• The copper strip is prepared for performing test. It is washed properly with
solvent (acetone) and surface of strip is prepared by rubbing with silicon
carbide grid paper.

• Clamp the strip with ice and polish it until uniform rubbing, when strip is
clean immerse it in prepared sample.

• The strip is kept into 30 ml of sample which is kept inside the test bomb and
the lid is screwed tight.

• After two hours in the bath the bomb is withdrawn and it is cooled with water.

• The bomb is opened, the test tube is taken out and carefully the strip is
withdrawn from the sample.

• The strip is compared with ASTM corrosion standards comparison chart and
report the tarnish level.

RESULT
 The corrosiveness of the given sample is found out using the copper strip and
comparing it with ASTM standards and its value is found to be ---------------------------
 CONGEALING POINT OF WAX

AIM

To determine the congealing point of given sample wax.

DEFINITION

Congealing point may be defined as the temperature of which molten petroleum wax when
cooled under prescribed conditions ceases to flow.

OUTLINE

A sample of wax is melted and droplet is made to adhere to the bulb of the thermometer.
Using a pre warmed flask as an air jacket, the droplet on the bulb is allowed to cool at a fixed
rate until it congeals. The congealing point is observed as the temperature at which the
droplet ceases to flow as the thermometer is turned.

APPARATUS REQUIRED

Thermometer, Erlenmeyer flask, Cork or Rubber stopper.

PROCEDURE

 The thermometer is adjusted through the stopper so that the bottom of the bulb will
be 10 to 15 mm above the bottom of the Erlenmeyer flask when the stopper is fitted snugly
in the flask.
 After making this adjustment, the thermometer and stopper are removed from the
flask, carefully without changing the position of the stopper relative to the thermometer stem.
 Approximately 50gm of sample is placed, which is representative of the material
under inspection in a porcelain evaporating dish or other suitable container.
 The empty Erlenmeyer flask is placed (without the thermometer assembly) and the
container holding the sample in a temperature-controlled oven set at 99 ± 3 0c (210 ± 50f)
until the sample and flask reach oven temperature.
 The sample is removed from the oven and the thermometer bulb is completely
immersed without covering any part of the thermometer stem with sample. The sample is
stirred gently with the thermometer until the mercury column has stopped rising.
 While holding the thermometer bulb in the molten wax sample, the heated flask is
removed from the oven, using a towel or gloves to project the hands. Now carefully the
thermometer from the sample adhering to the bulb is removed.
 The thermometer is held in a position firmly and is fit and stoppered into the flask.
The assembly is kept in a horizontal position.
 While the drop on the thermometer bulb is observed at an eye level position. The
thermometer and flask are rotated about a horizontal axis. a steady and even rate are used for
each continuous full revolution, and each revolution is completed in not less than 2 sec not
more than 3 sec.
 The completion of each revolution should not be paused any longer than required to
reindex the fingers for the next full and continuous rotation. When the drop is observed to
rotate with the bulb immediately the thermometer to the nearest 0.25 0c (0.50F) is read and
this determination is recorded.
 A repeat determination is made on the wax sample. If the variation of these two
determinations does not exceed 10c (20f) the average of these determinations is recorded as a
congealing point of the sample under test.
 If the variation of two determinations is greater the 10c (20c) additional reading is
recorded, and the average of the three determination is recorded as the congealing point.

SIGNIFICANCE

Congealing point is a wax property that is of interest to many petroleum wax consumers.
It indicates temperature at which sample when cooled under prescribed conditions develop a
se or resistance to flow. At that temperature the wax maybe at or close to the solid state or it
may be semisolid and quite unctuous depending on the composition of the wax congealing
property is associated with the formation of a gel structure as the sample cools.

RESULT

The average of the multiple determinations as the congealing point of the given sample