EXP.

NO: 1 RAMSBOTTOM CARBON RESIDUE OF PETROLEUM PRODUCTS

OBJECTIVE
The objective of this test is to determine the amount of residue resulting from evaporation and pyrolysis
of oil.

SIGNIFICANCE
Provides an indication of oil tendency toward coke formation.

APPARATUS
The apparatus consists of a glass-coking bulb, control bulb, sample charging syringe, metal control
furnace and temperature measuring device.

Ramsbottom Carbon Residue Apparatus

Coking Bulb

PROCEDURE
 A new glass-coking bulb is placed in the coking furnace that operates at 550 ºF for about 20 min
to remove any water, foreign or organic matters then dried in a closed dissector.
 The sample is weighed, heated if necessary to reduce it viscosity then introduced in the coking
bulb by means of hypodermic syringe.
 The coking bulb is weighed before placing it in the metal coking furnace.
 The sample is kept in the furnace at 550 ºF for about 20 min to vaporize the volatile materials and
allow the heavier residue to undergo cracking and coke formation.
 The bulb is then taken out, cooled in the dissector and weighed.
 The carbon residue is calculated by the same equation used in conradson carbon test.
CALCULATION

Weight of bulb, W1= 11.8gm

Weight of bulb with sample, W2= 14.39 gm
Weight of bulb with residue, W3= 12.1 gm
Volume of sample = 3 ml

Weight of the residue = W3-W1 gm

= 12.1 – 11.8
= 0.3 gm
Original weight of sample = W2-W1 gm
= 14.39 – 11.8
= 2.59 gm

𝑊𝑒𝑖𝑔 𝑕𝑡 𝑜𝑓 𝑡𝑕𝑒 𝑟𝑒𝑠𝑖𝑑𝑢𝑒

Percentage of carbon residue = ∗ 100
𝑂𝑟𝑖𝑔𝑖𝑛𝑎𝑙 𝑤𝑒𝑖𝑔 𝑕𝑡 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒
= (0.3/2.59)*100
= 11.58%

RESULT:
The percentage of carbon present in given sample 11.58 %.
 EXP. NO: 2 CONRADSON CARBON RESIDUE OF PETROLEUM PRODUCTS

OBJECTIVE
To determination the amount of carbon residue left after evaporation and pyrolysis of oil.

SIGNIFICANCE
It is applicable to relatively nonvolatile petroleum products (heavy) which partially decompose on
distillation at atmospheric pressure.

APPARATUS REQUIRED
Includes: burner, tripod, nickel-chrome triangle, refractory block, porcelain crucible, monel crucible and
cover; Skidmore crucible and cover-monel and a monel hood and bridge

PROCEDURE
 A sample is heated to about 50 ºC and shaken for 30 min. then filtered through a mesh screen.
 A 10 g sample is weighed (free of moisture & suspended matter) into a tarred porcelain or silica
crucible containing 2 glass beads 2.5 mm in diameter.
 The crucible is placed in the center of skidmore crucible which is set at the center of the iron
crucible and covers are applied to both of skidmore& iron crucible.
 A strong flame is applied from meker-type gas burner to have high heat for a period of 10 min.
 When smoke appears form the chimney the burner is moved or tilted to ignite the vapor then
removed temporarily.
 When the vapors cease to burn the heat is reapplied until the bottom of the sheet iron crucible is
cherry red.
 The burner is removed and the apparatus is cooled until no smoke appears then the cover of
skidmore crucible is removed (about 15 min)
 The porcelain or silica crucible is removed and placed in the desiccators, cooled and weighed and
the % of carbon residue is calculated based on the original sample.
CALCULATION

Weight of the crucible, W1= 24.3 gm

Weight of the crucible with oil, W2= 47.4 gm
Weight of crucible with residue, W3= 24.31gm
 Weight of the residue = W3-W1 gm
= 24.31 – 24.3
= 0.01gm

Original weight of sample = W2-W1 gm

= 47.4 – 24.3
= 23.1 gm

𝑊𝑒𝑖𝑔 𝑕𝑡 𝑜𝑓 𝑡𝑕𝑒 𝑟𝑒𝑠𝑖𝑑𝑢𝑒

Percentage of carbon residue =𝑂𝑟𝑖𝑔𝑖𝑛𝑎𝑙𝑤𝑒𝑖𝑔 𝑕𝑡 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒
∗ 100

= (0.01/23.1)*100
= 0.043%.

RESULT
The percentage of carbon residue in the given sample 0.043 %.
 EXP. NO: 3 VACCUM DISTILLATION
OBJECTIVE
To determine the distillation characteristics (boiling range) of the given sample using the
distillation apparatus.

SCOPE
This test method covers the distillation of natural gasoline, motor gasoline, aviation gasoline,
aviation turbine fuels, special boiling point spirits, naphtha, white spirit kerosene, gas oils, distillate fuel
oils and similar petroleum products, utilizing either manual or automated equipment.

PROCEDURE
 A 100 ml sample, placed in a flask, is heated in a regulated rate (so that a uniform average rate of
condensation in ml/min is maintained). This rate varied from zero to 5V% recovered, from 5 to
10 V% recovered and so on.
 When the first drop appears at the lower end of the condenser tube, the thermometer reading
(vapor temperature) is recorded as the initial boiling point (IBP).
 Temperature readings are recorded at several V% distilled (Table 1) up to the final boiling point
(FBP) and heating is discontinued.
 After the flask has cooled the volume of remaining liquid is measured and recorded as the
recovery.
 For heavy fractions, heating is discontinued when decomposition point is observed (the vapor
reaches a maximum temperature then starts declining before the end point).
RESULT
The distillation characteristics of the given sample is found and the graph also plotted.
 Exp. No: 4 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.

OBSERVATION

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

1 92.5 145 30.97

2 100 132 28.02
3 140 53 8.31

FORMULA

When t < 100 secs, v = 0.226t - 195/t Centistokes

When t >100 secs, v = 0.220t - 135/t Centistokes.
Calculation:
1. T = 92.50F, t = 145 sec
v = 0.220t - 135/t
v = (0.220*145) – (135/145)
v = 31.9 – 0.93
v = 30.97 cSt
 2. T = 100 0F, t = 132 sec
v = 0.220t - 135/t
v = (0.220*132) – (135/132)
v = 29.04 – 1.02
v = 28.02 cSt

3. T = 140 0F, t = 53 sec

v = 0.226t - 195/t
v = (0.226* 53) – (195/53)
v = 11.98 - 3.67
v = 8.31 cSt

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.
 Exp. No: 5 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 ---------------------------
 EXP. NO: 6 CLOUD AND POUR POINT

AIM:

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

APPARATUS REQUIRED:

 Constant temperature bath

 Thermometer
 Flat bottomed test tube

DEFINITION:

Cloud point:

The cloud point of petroleum is the temperature at which a cloud or haze of crystals appear at the
bottom of the test jar, when the sample is cooled under prescribed conditions.

Pour point:

Pour point is the lowest temperature expressed in multiples of 3 0C at which the oil is observed to
flow when cooled and examined under prescribed conditions.

THEORY:

The cloud point and the pour point are related to the flow conditions of crude and its products at
low temperature.

The cloud point gives the rough idea of the temperature above which the oil can be handled
safely, without any fear of congealing or filter clogging.

The pour point is determined to estimate the temperature at which a sample of oil becomes
sufficiently solid to prevent its movement by pumping.

The pour point temperature depends to a large extent on the thermal history of the sample. Also
the pour point indicates the waxy nature of the sample.

PROCEDURE:

 Oil is poured into the test jar up to the level mark of 51 to 57 mm. If necessary the oil is
heated until it is sufficiently enough to flow.
 The test jar is closed with the cork carrying the thermometer. The cork position is adjusted
to make it fit properly into the tube.
 The thermometer bulb is immersed so that the beginning of the capillary is 3mm below the
oil surface.
 The test jar surrounded by the air jacked is kept in the freezing mixture and it is allowed to
cool.
 The falling temperature was observed with every degree fall of temperature in the given
sample. The tube was withdrawn from the air jacket for a moment of about (2-3sec) and
examined. It was then replaced immediately.

 The temperature at which the cloudiness appeared was noted as the cloud point.
 The test tube was cooled continuously. The test tube was withdrawn often for 5 0C fall of
temperature to observe the flow or pour point of the sample.
 The temperature at which the oil does not flow in the tube even when kept horizontal for
5sec is recorded as pour point

SAMPLES SHOWING CLOUD AND POUR POINT

.
STANDARD POUR POINTS OF CRUDES USED IN INDIA

Sl.No. Crude name Pour point degC

1. Ankleshwar 18

2. North/Gujarat 27

3. Bombay high 30

4. Basrah -15

5. UMM Shaiff -15

6. High speed diesel 6

Observation:

Sample Cloud Point, ̊C Pour Point, ̊C

A 23 11

B 14 2

C 23 14

D 20 8

RESULT:

Thus the cloud and pour point of the given sample was found.