Practical Workbook

ACH-612 PETROLEUM AND PETROCHEMICALS

Name:

Year:

Roll No:

Batch:

Discipline:

DEPARTMENT OF APPLIED CHEMISTRY AND CHEMICAL

TECHNOLOGY
UNIVERSITY OF KARACHI
 CERTIFICATE

It is Certified that Mr. / Miss

__________________, student of
class ___________,
batch_____________, and bearing
roll no. __________________ has
completed his/her Lab work in the
subject of CH-612 Petroleum and
Petrochemicals as prescribed and
approved by the Department.

_____________
Course Teacher
 Lab Sessions

Sr No OBJECTIVE

01 To determine the relative density OR specific gravity of a liquid sample by hydrometer

02 To determine the relative density of a liquid sample by Relative Density Bottle.

To determine the viscosity of a liquid sample by Cannon-Fenske Opaque (Reverse-Flow)

03
Viscometer.

To determine “FLASH POINT” of a given samples by “CLEVLEND OPEN CUP

04
TESTER”

05 To determine the carbon residue of given sample.

06 Lovi Bond Color test.

07 To determine the sulphated ash content of given sample.

08 To determine the acid number.

 Lab Session 01
OBJECTIVE:
To determine the relative density OR specific gravity of a liquid sample by

hydrometer

INTRODUCTION:

A hydrometer is an instrument used to measure the specific gravity (or relative

density) of liquids; that is, the ratio of the density of the liquid to the density of
water.

A hydrometer is usually made of glass and consists of a cylindrical stem and a

bulb weighted with mercury or lead shot to make it float upright. The liquid to be
tested is poured into a tall container, often a graduated cylinder, and the
hydrometer is gently lowered into the liquid until it floats freely. The point at which the surface of the liquid
touches the stem of the hydrometer is noted. Hydrometers usually contain a scale inside the stem, so that
the specific gravity can be read directly.
PRINCIPLE:

Operation of the hydrometer is based on Archimedes' principle that a solid suspended in a fluid will be
buoyed up by a force equal to the weight of the fluid displaced by the submerged part of the suspended
solid. Thus, the lower the density of the substance, the farther the hydrometer will sink.
PROCEDURE:

1. Find the suitable hydrometer, which do not completely sinks in the graduated cylinder.
2. Immerse it properly, do not put it in such a way that it strikes hard on the base of graduated
cylinder.
3. Give it some time to stabilize.
4. Note down the meniscus reading.
OBSERVATIONS AND CALCULATIONS:

1. Room Temperature = _________________

2. Specific gravity of Liquid Sample 1 = _____________________
3. Specific gravity of Liquid Sample 2 = _____________________
4. Specific gravity of Liquid Sample 3 = _____________________

API Gravity Calculation:

RESULTS:

Relative density OR Specific gravity of the given samples are found to be

 Lab Session 02
OBJECTIVE:

To determine the relative density of a liquid sample by Relative Density Bottle.

INTRODUCTION

Density determination by Relative Density Bottle is a very precise method. It uses a working liquid
with well-known density, such as water. The Relative Density Bottle is a glass flask with a close-
fitting round glass stopper. This allows for obtaining a given volume of measured and/or
working liquid with a high accuracy.

METHODOLOGY

First we fill Relative Density Bottle with distilled water. According to equation, the volume of
water that is filling is

We repeat the procedure for the liquid with unknown density and determine its weight (measured
weight minus weight of empty Relative Density Bottle). Volume V obtained in this measurement
is the same as the volume of water determined from equation.

Combining above equation yield

Yields a relation that provides the density of measured liquid

Or specific gravity of liquid is simply =

CALCULATIONS AND RESULTS:

 Lab Session 03
OBJECTIVE:
To determine the viscosity of a liquid sample by Cannon-Fenske Opaque
(Reverse-Flow) Viscometer.

PRINCIPLE:

This test method specifies a procedure for the determination of the kinematic viscosity
of liquid petroleum products, both transparent and opaque, by measuring the time for a
volume of liquid to flow under gravity through a calibrated glass capillary viscometer.
The dynamic viscosity can be obtained by multiplying the kinematic viscosity by the
density of the liquid.
Viscometers are calibrated at different temperatures.

Kinematic Viscosity is calculated as

V=Ct (mm2/sec)

Where, C- viscometer constant (mm2/sec)/sec

t- flow time (sec)

METHODOLOGY & PROCEDURE:

1. Clean the viscometer using suitable solvents, and dry by passing clean, dry,
filtered air through the instrument to remove the final traces of solvents. Periodically, traces of
organic deposits should be removed with chromic acid or non-chromium cleaning solution.
2. If there is a possibility of lint, dust, or other solid material in the liquid sample, filters the
sample through a fritted glass filter or fine mesh screen.
3. To charge the sample into the viscometer, invert the instrument and apply suction to tube
arm L, immersing tube N in the liquid sample, and draw liquid to mark G. Wipe clean
arm N, and turn the instrument to its normal vertical position.
4. Place the viscometer into the holder, and insert it into the constant temperature bath.
Align the viscometer vertically in the bath.
5. Allow sample to flow through capillary tube R and approximately half-fill bulb A,
stopping the meniscus in bulb A by placing a rubber stopper in tube N (you may prefer to
stopper tube L for larger size tubes).
6. Allow approximately 10 minutes for the sample to come to bath temperature at 40°C and
15 minutes at 100°C. Make sure the meniscus in bulb A does not reach line E.
7. Remove the rubber stopper and allow the meniscus to travel upwards into bulb C,
measuring the efflux time for the meniscus to pass from mark E to mark F.
 8. Calculate the kinematic viscosity of the sample by multiplying the efflux time in seconds
by the viscometer constant for bulb C.
9. The same procedure will follow for Upper bulb (J)
CALCULATIONS AND RESULTS
 Lab Session 04
OBJECTIVE:

To determine “FLASH POINT” of a given samples by “CLEVLEND OPEN CUP TESTER”

INTRODUCTION:

This flash point and fire point test method is a dynamic method and depends on definite rates of
temperature increases to control the precision of the test method. Its primary use is for viscous
materials having flash point of 79°C (175°F) and above.

Flash point values are a function of the apparatus design, the condition of the apparatus used, and
the operational procedure carried out. Flash point can therefore only be defined in terms of a
standard test method, and no general valid correlation can be guaranteed between results
obtained by different test methods, or with test apparatus different from that specified.

PRINCIPLE:

Standard Test Method for Flash point by Cleveland Open Cup Tester. The flash point is one
measure of the tendency of the test specimen to form a flammable mixture with air under
controlled laboratory condition.

PROCEDURE:

1-Fill the test cup with the sample so that the top of the meniscus of the test specimen is level
with the filling mark, and position the test cup on the center of the heating plate.

2-Light the test flame and adjust it to a diameter of 3.2 to 4.8 mm (1⁄8 to 3⁄16 in.) or to the size of
the comparison bead, if one is mounted on temperature measuring device increases 5 to 17°C (9
to 30°F)/min.

3-Apply heat initially at such a rate that the temperature as indicated by the temperature
measuring device increases 5 to 17°C (9 to 30°F)/min

4-Apply the test flame when the temperature of the test specimen is approximately 28°C below
the expected flash point and each time thereafter at a temperature reading that is a multiple of
2°C. Pass the test flame across the center of the test cup at right angles to the diameter, which
passes through the temperature measuring device.

5-Record, as the observed flash point, the reading on the temperature measuring device at the
time the test flame causes a distinct flash in the interior of the test cup.
OBSERVATION:

S.NO NO.OF SAMPLES FLASH POINT TEMPERATURE °C

1
2
3

CALCULATION AND RESULTS:

Flash point of a given samples by cleveland open cup tester are found to be
Lab Session 05
Lab Session 06
 Lab Session 07
OBJECTIVE:

To determine the suphated ash content of given sample.

INTRODUCTION:

The sulfated ash test utilizes a procedure to measure the amount of residual
substance not volatilized from a sample when the sample is ignited in the presence
of sulfuric acid.

The test is usually used for determining the content of inorganic impurities in an
organic substance.

PROCEDURE:

1. Heat 10gm sample in crucible until only ash and carbon left.
2. Cool an then add concentrated sulphuric acid drops to moist the residue and
place it at the hot plate until fumes are no longer evolved. (or intensity of
fumes becomes very low)
3. Place the dish in furnace at 300oC, gradually increase temperature to 550oC,
and continue heating until oxidation of carbon is practically completed.
(Around 10 to 15 minutes).
4. Allow the dish to cool to room temperature; we can use desiccator as well.
5. Add diluted sulphuric acid (2 to 3 drops water and 4 to 5 drops sulphuric
acid) to moist the entire residue again.
6. Carefully heat the dish in the hot plate until fumes are no longer evolved.
7. Again place the dish in furnace at 300oC, gradually increase temperature to
775oC, and continue heating around 10 to 15 minutes.
8. Allow the dish to cool to room temperature using desiccator and weigh it.

CALCULATION:

Calculate the sulphated residue of the sample as follows:

Sulphated residue , percent = w/W *100

WHERE,

w- grams of residue

W- grams of sample

RESULT:
 Lab Session 08

OBJECTIVE:

To determine the Acid number of given sample.

INTRODUCTION:
Acid number is the measure of acidic substances in the oil under consideration. This number is
used as a guide in quality control of lubricating oil. It is also used as a measure of lubricant
degradation.

PROCEDURE:
1. Make a solution of 0.1M KOH in flask. (0.6 gm KOH in 100 ml of isopropyl alcohol)
2. Take this solution in burette.
3. Take a conical flask, add 20 gm sample in it. And also add 100 ml solvent. The solvent
recipe contains 50 ml toluene, 0.5 ml water and 49.5 ml isopropyl alcohol.
4. Add 0.5 ml of indicator in the flask. (indicator is para-naphtholbenzein)
5. Without delay start titration with the 0.1 M KOH solution present in burette.
6. The yellow orange colour of the solution changes to green when the reaction is
neutralized.
7. Also take a blank reading without sample following the same procedure, this reading will
be used in calculation.

CALCULATION:
Calculate the acid number as follows:

Acid Number (mg of KOH/gm) = [(A – B) M x 56.1] / W

Where,

A= KOH solution required for titration of the sample, ml

B= KOH solution required for titration of the blank, ml

M= molarity of KOH solution, M

W= sample used, gm
RESULT: