University of Technology

Chemical Engineering Department

Lecturer Layla Abdul-Rahman

Lecturer Tagreed Lutfee

Asst.Lecturer Basheer Ahmed

Supervision By

Lecturer Dr. Intisar hussain

2012
 Index

No. Experiment Page

No.

1 ASTM Distillation 1

2 Viscosity 5

3 Ash From Petroleum Products 10

4 Flash and Fire point 12

5 Gum and Gum Stability 15

Conradson Carbon Residue of
6 18
Petroleum
7 Density and Specific Gravity 20

8 Water Content in Crude Oil 25

 Experiment No.1

ASTM Distillation
1-Introduction:-

The distillation tests give an indication of the quality of the

products that can be obtained from petroleum, and the tests are used to
compare different petroleum types through the yield and quality of the
300°C (572°F) residuum fraction.
The basic method of distillation (ASTM D-86) is one of the oldest
methods in use because the distillation characteristics of hydrocarbons
have an important effect on 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 petroleum and derived
products during storage and use. Volatility is the major determinant of the
tendency of a hydrocarbon mixture to produce potentially explosive
vapors. Several methods are available to define the distillation
characteristics of petroleum and its various petroleum products.

2-Object:-
To find the relation between the vol. percentage of distilled cuts and
its boiling range.

3- procedure:-
1- A (100ml) sample is distilled under prescribed conditions which
are appropriate to its nature. Systematic observation of
thermometer readings and volume of condensate are made, and
from these data, the results of the test are calculated and
reported.
 Experiment No. 2

Viscosity
Introduction

Viscosity describes a fluid's internal resistance to flow

Viscosity coefficients can be defined in two ways:

 Dynamic viscosity, also absolute viscosity, the more usual one

(typical units Pa·s, Poise, P);
 Kinematic viscosity is the dynamic viscosity divided by the density
(typical units cm2/s, Stokes, St).

Kinematic viscosity is a measure of the resistive flow of a fluid under

the influence of gravity. It is frequently measured using a device called a
capillary viscometer — basically a graduated can with a narrow tube at
the bottom. When two fluids of equal volume are placed in identical
capillary viscometers and allowed to flow under the influence of gravity,
a viscous fluid takes longer than a less viscous fluid to flow through the
tube. Capillary viscometers are discussed in more detail later in this
section.

Object

To determine the viscosity of different oil products by using the

viscometer.
 Experiment No. 3

Ash From Petroleum

Introduction:-

Petroleum, as recovered from the reservoir, contains metallic

constituents but also picks up metallic constituents during recovery,
transportation, and storage. Even trace amounts of these metals can be
deleterious to refining processes, especially processes in which catalysts
are used. Trace components, such as metallic constituents (Nickel and
vanadium along with iron and sodium are the major metallic constituents
of crude oil) can also produce adverse effects in refining either (1) by
causing corrosion or (2) by affecting the quality of refined products.

1-Object
To set the percentage of ash in crude oil

1- Procedure:-
1- Heat evaporating dish of crucible at 100Cofor 10 min .Cool to
room temp in a suitable container.
2- Weigh in to the dish of crucible (10) gm of sample.
3- Burn the sample by a flame maintain at such a temp that the
sample continues to burn at a uniform rate, leaving only ash and
carbon.
4- Heat the residue in the furnace at 775Co until all carbonaceous
material has disappeared. Cool the dish to room temp in a
suitable container and weigh.

10
 Experiment No. 4

Flash and Fire point

1- Introduction

Flash point is the minimum temperature at which the vapour from

oil sample will give a momentary flash on application of a standard flame
under specific test condition. Signification of the flash point is that it can
predict the possible fire hazards during transportation, storage and
handling. Early tendencies were to incorporate more volatiles in
kerosenes, thus inviting unusual fire hazards.

Fire point closely follows the flash point. The test is carried out in open
cup rather than a closed one. Cleveland apparatus (ASTMD92) offers the
advantage of open flash point and fire point. Fire point temperature is
noted when the oil vapours can burn continuously for 5 second when
tested in flash point apparatus and it occurs after the flash point, by
3-4Co.For domestic needs a very high flash point above 50 Co is also not
desirable . The easy ignition is credited to volatiles only and decrease in
volatiles enhances the flash point causing difficulty in ignition.

2- Object:-

To set the flash point and ignition point of petroleum products

according to degree of volatility use one of the following methods:-

* Abel test

Used to set the flash point of the products that are relatively light,
ranging between points (18 -71) Co.

12
 Experiment No.5

Gum and Gum Stability

Introduction

Cracked gasoline contain olefins and are on the whole not so stable
as those obtained by direct distillation, the olefin especially those having
more than one double bond per molecule , show a tendency to combine
with atmospheric oxygen and polymerize; high molecular resinous
substance known as gum are there by formed. They contain organic
peroxide group and their formation is autocatalytic; some time is needed
for the first small amount of peroxides to be formed and the process then
continues at an increasing rate.

Gum in gasoline has several harmful consequences. It may be

deposited in various parts of the engine for example in the manifold or on
the valves, where it may be cause mechanical trouble.

Since the refiner or the consumer of gasoline has to consider as possible

deterioration of his product in storage, he will wish to know not only (a)
the amount of gum present at the time of testing [a quantity know as gum]
but also (b) the change in gum content with time i.e. gum stability.

Existent gum is now determined by an accelerated evaporation of

the gasoline in a current of air or steam several tests are available; they
chiefly differ in the temperature employed. Modern practice seems to
prefer a high temperature.

The test used at present for estimating the tendency to gum

formation on storage consist, in heating a sample of the gasoline in an
 Experiment No.6

Conradson Carbon Residue of

Petroleum
Introduction

Conradson carbon residue is finding use to characterize heavy

residue fuels, coker feed stocks, which can not readily be leaded into a
rams bottom coker bulb, and when it is desirable to examine or further
test the residue.

Summary of method

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 a disccator and weighed. The residue remaining is
calculated as a percentage of the original sample, and reported as
conradson residue.

Object:-

To determine the carbon residue by using Conradson method

Apparatus:

The apparatus shall consist of the following:-

1- Porcelain crucible.
2- Iron crucible – skidmore iron crucible.
3- Iron crucible – spun sheet iron.
 Experiment No.7

Density and Specific Gravity

Introduction

1. This method covers the determination of the density of crude

petroleum and petroleum products or mixtures of petroleum and
non petroleum products normally handled as liquids. The method is
restricted to liquids having Reid vapour pressures of 1.25 bar
(18.5lbf) or less and having viscosities less 50 c.st. at the test temp.
2. Special precautions are described for determining the density of
highly volatile liquids.
3. The method is recommended for the accurate determination of the
density of all except the more viscous products, and is particularly
useful when only small amount of sample are available.
Definition
a- Density for the purpose of this method is the mass (weight in
vacuo) of liquid per unit volume at 15Co. When reporting results,
explicitly state the density in units of mass and volume, together
with the standard reference temp. as g/ml at 15Co
b- Relative density for the purpose of this method is the ratio of the
mass of a given volume liquid at 60 oF to the mass of an equal
volume of pure water at the same temp. when reporting results
explicitly state the standard reference temp, ex. relative density
15/15Co
c- API gravity, a special function of relative density 15/15Co, is
represented by
 Experiment No.8

Water Content in Crude Oil

Introduction:-

Contamination in residual fuel oil may be indicated by the presence

of excessive amounts of water, emulsions, and inorganic material such as
sand and rust. Appreciable amounts of sediment in a residual fuel oil can
foul the handling facilities and give problems in burner mechanisms.
In any form, water and sediment are highly undesirable in fuel oil,
and the relevant tests involving distillation (ASTM D-95), centrifuging
(ASTM D-96), extraction (ASTM D-473), and the Karl Fischer titration
(ASTM D-4377) are regarded as important in determination of quality.
Object:-
To calculate the amount of water in crude oil and petroleum product by
Karl-Fisher titration.

Experimental work:-
1- Apparatus :-
The apparatus comprises a glass or metal still a heater, a reflex condenser,
and a graduated glass trap, the still, trap and condenser may be connected
by any suitable method for producing a leak-proof joint.

2- Solvent – carrier liquid

Any suitable hydrocarbon boiling in the (100 -200)Co range may be used,
as toluene , xylene ,(toluene &xylene ,volatile hydrocarbons which are
absorbed by inhaling the vapour or through the skin by contact with the
liquid , use adequate ventilation and avoid skin contact ).
References
1- Standard methods for analysis and testing of
petroleum and related products(1990)
Vol.1&2; Institute of petroleum, London- IP

2- Francis & peters, "Fuels & Fuels Technology", 2nd

SI edition, 1980.

3- J.H.Van der Have,C.G.Verver, " Petroleum and its

Products", Sir ISAAC Pitman & sons,Ltd,1957

4- Internet.