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Fuel & Refinery Lab.

Experiments guide
2023
A guide to all lab experiments for 2023

1
 Content table
Exp. NO. Exp. Name Page NO.

1 ASTM Distillation 3

2 Viscosity 10

3 Ash From Petroleum 16

Products
4 Flash point and fire 21
point Definitions
5 Conradson Carbon 27
Residue
6 Density and Specific 32
Gravity

2
 Experiment NO.

1
ASTM Distillation

3
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.

4
5
Object:-
To find the relation between the vol. percentage of distilled cuts and
its boiling range.

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.
2- Fill the condenser box to cover the condenser tube with any
non-flammable coolant which is suitable, such as chopped ice, water,
brine or ethylene glycol solution. If chopped ice is used, add
sufficient water to cover the condenser tube.
3- Remove any residual liquid in the condenser tube, by swabbing
with a piece of soft, lint- free cloth attached to acord or copper
wire.
4- Measure (100ml) of sample in a graduated cylinder and transfer
it as completly as practicable to the distillation flask, taking care
that non of the liquid flows in to the vapour tube.
5- Fit the thermometer provided with a sung fitting , well-rolled
cork , tightly into the neck of the flask so that the bulb is
centered in the neck and the lower end of the capillary is level
with the highest point on the bottom on the bottom of inner
wall of the vapor tube . as shown in fig. 1

6
6- Place the flask containing the charge in its support; and by
means of a cork through which the vapour tube has been passed,
make a tight connection with the condenser tube. Adjust the
flask so that it is in a vertical position, and so that the vapour
tube extends into the condenser tube for a distance of 1 to 2 inch
(25-50mm).

7- Place the graduate that was used to measure the charge, without
drying, into its bath, under the lower end of condenser tube so
that the end of the condenser tube is centered in the graduate
and extends therein for a distance of at least 1 inch (25mm), but
not below the 100ml mark.
8- Apply heat to the distillation flask and contents .After observing
the initial boiling point move the graduate so that the tip of
condenser touches its inner wall. Continue to regulate the
heating so that the rate of condensation into the graduate shall
be uniform

7
Fig.2 Apparatus assembly using gas burner.

8
 4- Calculation:-
1- Prepare table of data as follow:-

Temp. Co %distilled Density 𝝆

I.B.P o 𝜌1
T1 5% 𝜌2
T2 10% 𝜌3
T3 15% 𝜌4

End pt. 100% 𝜌n

2- Plot relation between Temp Co & %distilled

E.B.P.
Temp.

I.B.P

0 5 10 100%

%dis.

5- Discussion:-
1- Compare your result with the reference.
2- Explain your observation if the process is continuous.
3- Compare between different distillations

9
Experiment NO.

2
Viscosity

10
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

11
Types of Viscometers
a) Redwood viscometer

Fig.1 Detail of Redwood viscometer

b) Saybolt Viscometer

Fig.2 Detail of Saybolt viscometer

12
c) U-tube Viscometer

Principle of method

U-tube glass viscometers (as shown in Fig.3) allow an accurately

reproducible volume of liquid to pass through a capillary at a constant
temperature by the application of an accurately reproducible force. The time
taken for a liquid to flow is proportional to the ratio of the dynamic
viscosity to the density of the fluid, hence to its kinematic viscosity. The
constant of proportionality for the instrument is obtained by carrying out a
determination in the viscometer with a fluid of known viscosity. The
kinematic viscosity of a fluid viscosity greater than 10 centistokes is given
by the expression.

A filtered sample of the oil under test is introduced into the viscometer by
suction or by pipetting into the wide tube (Fig.4) so that air bubbles are
absent and the level of oil stands a few millimeters above the level E. The
viscometer is then placed in a thermostat, maintained at the required
temperature, and adjusted so that it is exactly vertical. After a time, varying
from 20 min for temperatures near the normal to 30 min at

100Co, the oil is blown or sucked into the tube A to a point 1cm above the
etched level B. The oil is thin and allowed to flow freely back down the
capillary, taking the time of fall from mark B to mark C by means of an
accurate stopwatch reading to 1/5 sec. the experiment is repeated until
duplicate tests are repeatable within 0.2%.

13
Fig.3 Types of viscometers Fig.4 U-tube viscometer

Chemicals and materials:

1- Kerosine

2- Gasoil

3- Beaker

4- U-tube viscometer

5- Pipet

Procedure:

1- Use a Clean and dry viscometer.

2- Put a certain amount of liquid in the large bulge viscometer and pull it by
pipette until the small bulge is full.

3- Put the viscometer vertically in the stand.

4- Let the liquid flow through the capillary tube with run time when

the liquid reaches the mark shown on the viscometer and then stop

time when the liquid reaches the bottom mark.

5- Repeat the experiment with other liquids.

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Calculation:

Calculate the viscosity by the relationships:

1- For Kinematic viscosity:

𝑣 = 𝐶𝑡
𝑣 = viscosity

C = is the viscometer constant

t = time of flow in seconds

2- For Dynamic viscosity:

𝑣 = kinetic viscosity 𝑣 =µ/ρ

µ= dynamic viscosity

ρ = density of the substance

Discussion

1- What is the important variable that the viscosity depends on ...explain

2- Discuss the results and compare them with standard values from reference.

References

1- [Link]
kinematic-viscosity

2- Data source: Viswanath D.S, Ghosh T.K., Prasad D.H. L., Dutt
N.K. and Rani K.Y., (2007), “Viscosity of Liquids: Theory,
Estimation, Experiment, and Data”, Springer, P.O. Box 17,
3300 AA Dordrecht, The Netherlands.
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 Experiment NO.

3
Ash From Petroleum Products

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Objectives
To determine the ash percentage in a sample of crude oil.

1. Introduction
Ash contents are defined as the inorganic residue that remains after the
combustion of crude oil in the air at a specified high temperature. These are
inorganic, non-combustible materials that can cause different types of
problems. Some of the components that contribute to ash formation are found
naturally in crude oil; others are present as a result of refining or
contaminated during transportation and storage. For example, petroleum, as
recovered from the reservoir, contains metallic constituents but also picks up
metallic constituents during recovery, transportation, and storage. These
metallic constituents are the main elements of ash-forming including
vanadium, sodium, calcium, magnesium, zinc, lead, iron, sodium, and nickel
which can be deleterious to refining processes, especially processes in which
catalysts are used (i.e., catalyst deactivation whether it be by physical
blockage of the pores or destruction of reactive sites). At higher levels of ash
content, crude oil has a greater propensity to create sludge or sediment which
can cause adverse effects in refining either by causing corrosion or affecting
the quality of refined products. Therefore, methods have been developed for
counteracting the effects of ash. These include the use of additives,
modifications in equipment design, and the application of petroleum
processing methods such as water washing. An important point to remember
is that high-ash crude oils are those with an ash content of more than 0.05%,
whereas low-ash crude oils are those with an ash content of less than 0.02%
[1,2].

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2. Tools and materials
As seen in Figure 1, tools employed in this experiment include (1)
crucible (or lid) which is a vessel used to burn a sample of crude oil that
requires a high degree of heat; (2) digital balance; (3) tripod stand and
forceps; (4) bunsen burner as a source of flame which is a type of gas burner
used to combust a sample of crude oil on high heat; (5) furnace; and (6)
desiccator. Crude oil is the material that was employed in this experiment.

Figure 1. Instruments used in this experiment.

3. Procedure
As shown in Figure 2, the procedure employed to carry out this
experiment has several steps as follows:
1. First, we took a crucible and weighed it using a digital balance and
then, recorded the empty crucible's weight, which is W1.
2. Add a certain weight of a sample of crude oil to the crucible and then,
record the test sample's weight, which is W2.
3. Place the crucible containing the sample on the stand, light the burner
underneath it, and carefully heat it to a certain temperature so that

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 the sample continues to burn at a uniform rate, leaving only ash and
carbon when the burning stops.
4. Heat the residue in a furnace at 775 °C until all carbonaceous
materials have disappeared.
5. Cool the crucible in a desiccator at room temperature and then,
recorded this crucible's weight, which is W3.

Figure 2. Steps used in implementing this experiment.

4. Calculation
1. Measure the weight of the empty crucible (W1).
2. Measure the weight of the test sample and crucible (W2).
3. Measure the weight of the test sample after burn and crucible (W3).
4. Calculate the ash content as a weight percentage in the original crude
oil sample employing Eq. (1), as follows.
WA
Ash percent% = × 100 (1)
WS

19
where WS is the test sample weight (W2 − W1 , g) and WA is the ash weight
(W3 − W1 , g).

5. Discussion
1. Compare the results obtained with the references.
2. Why is this experiment carried out in the presence of air and can it
be carried out in isolation from air? Explain that
3. What issues arise when burning crude oils with a high ash content?
4. Why do petroleum products with light fractions have so little ash
content?
5. What are the disadvantages of the presence of sodium and vanadium
when heating fuel that contains these elements?

6. Reference
1. Speight, J. G. (2013). Enhanced recovery methods for heavy oil and tar sands,
Elsevier.
2. Speight, J. G. (2019). Heavy oil recovery and upgrading, Gulf Professional
Publishing.

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 Experiment NO.

4
Flash point and fire point
Definitions

21
Introduction

Flash point: is the lowest temperature at which the vapor of the test
specimen starts to ignite, but it does not sustain under the specified
conditions of the test.

Fire point: is the temperature at which the vapor will keep burning after
the ignition source is removed, Fire point is typically higher than the flash
point.

Significance of the Test

1. Flash point can be used to measure the tendency of the material to

catch flames. It is one of the properties which can be used to assess
the overall flammability of the material.
2. Flash point is used to class flammable and combustible materials
according to safety regulations.
3. Flash point can be used to obtain an idea about the presence of
volatile and flammable substances in a, theoretically, non-flammable
material.
4. Fire point is used to measure combustibility of the material.

Methods:

a. Abel test
Used to set the flash point of the products that are relatively light,
ranging between points (18 -71) oC
b. Pensky – Martens
Used to set the flash point of relatively heavy products, that the flash
point for it more than 71 oC
c. Cleveland test:-
Is used to test the flash point of heavy petroleum products.
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Apparatus and Equipment:

The main apparatus is called the Cleveland Open Cup Apparatus, shown in
Figure1. It consists of the following:

1. Test cup

2. Heating plate.

3. Test flame.

4. Thermometer capable of measuring

high temperatures up to 500°C

Figure (1) Cleveland open –cup flash

Sample Preparation:

1. Make sure that the sample is fluid. If the sample is not fluid, then heat
it carefully making sure that the temperature does not exceed
60ºC below the probable flash point.
2. Fill the cup with the sample to the specified level. Take care not
tooverfill the cup.

3. Air bubbles or foams should be carefully removed. Make sure that

thesurface is foam or air bubble-free surface before starting the test.
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 4. If foam could not be removed, then discard the sample completely
and prepare a new one.
Procedure:

1. Let the apparatus stand on a leveled

steady place. Protect from strong
sunlight.

2. Wash the test cup carefully using some solvent in order to remove
any traces of oils or residuals.

3. Support the thermometer in a vertical position. Locate the

thermometer halfway between the center and the side of the cup.

4. Fill the cup with the sample to the specified level. Take care not to
over fill the cup. Air bubbles or foams should be carefully removed
as mentioned earlier.

5. Light the test flame adjusting the flame to a diameter of 3 to 5 mm.

6. Start heating the sample with a relatively high speed (14ºC to 17ºC
per minute). Continue until the temperature is about 60ºC below
the probable flash point then decrease the heat so that the rate of
heating is about 5ºC to 6ºC per minute.

7. When the temperature is about 30ºC below the probable flash point,
apply the flame to the sample. The flame should be passed along the
center of the sample and also about the circumference in a smooth
way. The flame must be at a distance of not more than 2 mm above
the plane of the edge of the can. Watch for possible ignition. The
passing of the flame across the cup should be in about one second.

8. Repeat step 7 every increase of 2ºC.

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 9. Record the temperature at which flash ignition occurs. Record this
value as the flash point.

[Link] heating with the same rate (5ºC to 6ºC per minute) and
repeat steps 7 and 8.

[Link] the temperature at which ignition occurs and burning

continues. Record this value as the fire point of the tested material.

Results:

Record the degree of flash and fire points of each product then
compare results with standard values from reference.

Discussion:-

1. What in the importance of selecting the flash point and fire point
for oil products?

2. Could these apparatus be used for selecting flash and fire point
for air craft fuel and auto mobile fuel?

Figure (2) explain different flash point and fire point

25
References:

D 1310 Test Method for Flash Point and Fire Points of Liquids by
Tag Open-Cup Apparatus
D 4057 Practice for Manual Sampling of Petroleum and Petroleum
Products
D 4177 Practice for Automatic Sampling of Petroleum and Petroleum
Product

26
 Experiment NO.

5
Conradson Carbon Residue

27
Object:-
To determine the carbon residue by using Conradson method

Introduction
The Conradson Carbon Residue (CCR) test is a method used to determine
the amount of carbon residue left behind when a sample of crude oil is
distilled at high temperatures. The test provides an indication of the coke-
forming capacity of petroleum fraction or crude oil. In general, the test is
applicable to petroleum products that are relatively non-volatile, and which
decompose on distillation at atmospheric pressure.

The Conradson Carbon Residue is also an indicator of the relative

“heaviness” or “lightness” of crude oil, with higher values indicating a
heavier crude oil with a higher proportion of heavy, high-boiling point
hydrocarbons. Heavy crude oils typically have a higher Conradson Carbon
Residue value than light crude oils.

Conradson Carbon Residue is an important quality parameter of furnace oil,

showing the tendency of deposits on the burner tips.

• Diesel fuel deposits on the combustion chamber of diesel engine.

• For delayed cokers, the Conradson Carbon Residue estimation of coke
production
• CCR depicts the coke formation on the catalysts of Fluid Catalytic
Cracking Units and other catalytic units in petroleum refineries.
• CCR (Conradson Carbon Residue) values of arab crudes are; Arab Extra
Light 3.65 %, Arab Light 3.83%, Arab Medium 5.71%, and Arab Heavy
7.86 %.

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 Koehler Conradson Carbon Residue Apparatus

Summary of method
A quantity of sample is weighed, placed in a crucible, and
subjected to destructive distillation at a high temperature ~ 525 °C
and at atmospheric pressure. During a fixed period of severe
heating, the residue undergoes cracking and coking reactions. At
the end of the heating period, the crucible containing the
carbonaceous residue is cooled in a desiccator and weighed. The
residue remaining is calculated as a percentage of the original
sample and reported as Conradson carbon residue .

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Apparatus:
The apparatus shall consist of the following:-

1. Porcelain crucible.
2. Iron crucible – skidmore iron crucible.
3. Iron crucible – spun sheet iron.
4. Wire support.
5. Hood.
6. Burner.

Procedure
- Shake thoroughly the sample to be tested, first warming if necessary.
- Weigh to the nearest 5 mg, a 10 gm sample of the oil to be tested.
- Apply heat with a high, strong flame. Heat may be increased, if
necessary, when the flame does not show above the chimney, the
period of burning the vapours shall be 13± 1 min.
- Remove the burner and allow the apparatus to cool until no smoke
appears, and then remove the cover of the skidmore crucible (15min).
Remove the porcelain or silica crucible with heated tongs, place in the
desiccators, cool, and weigh. Calculate the percentage of carbon
residue on the original sample.

Calculation:-
Calculate the carbon residue of the sample or of the
10%distillation residue as follows:-

A=mass of carbon residue, in grams

W=mass of sample, in gm
𝐴∗100
% 𝑐𝑎𝑟𝑏𝑜𝑛𝑟𝑒𝑠𝑖𝑑𝑢𝑒 =
𝑊

30
Discussion:
1- If Compare the results with the standard vales from references.

2- Explain this property in the combustion process.

References

1. www, [Link]
2. [Link]
Engineering/Abdel-Aal-Alsahlawi/p/book/9781466506664
[Link]
apparatus-psc4711961

31
 Experiment NO.

6
Density and Specific Gravity

32
 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 [Link]. 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

No statement of reference temp. Is required, since 15Co is included in the

definition
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 Object:

To determine the standard density of oil and oil products by use the following
methods:

1- Hydrometer method
2- pyknometer method

Procedure:-

1- Density by hydrometer:
The hydrometer method is most suitable for determining the density,
relative density, or API gravity of mobile transparent liquids. It can also be used
for viscous oils by allowing sufficient time for the hydrometer to reach
equilibrium, or for opaque oils by employing a suitable meniscus correction.

Sample is brought to the prescribed temp. and transferred to cylinder

at approximately the same temp. The appropriate hydrometer lowered into the
sample and allowed to settle. After equilibrium has been reached; the hydrometer
scale is read, and the temp. of the sample is noted. If necessary the cylinder
and its contents are placed in a constant temp. bath to avoid excessive temp.
variation during the test.
a) Hydrometer of glass, graduated in unit density ,relative density , or APT
gravity as required
b) Thermometers
c) Hydrometer cylinder of clear glass, plastic, or metal. For convenience in pouring,
the cylinder may have a lip on the rim. The inside diameter of the cylinder
shall be at least 25mm greater than the outside diameter of the floats in the
sample with at least 25mm clearance between the bottom of the hydrometer and
the bottom of the cylinder .
d) Constant temp. bath for use when the nature of the sample requires a test
temp. much above or below room temp.
34
Fig 1. Hydrometer method

35
2- Density by pyknometer

The liquid sample is drawn into the pyknometer and after it has reached
equilibrium at the test temp. the liquid levels are noted and the pyknometer is
weighed . The density of the sample is them calculated from its weight, a
calibration factor proportion to an equal volume of water and a term which
correct for the buoyancy of air.

Ρ= w/v
Where:
Ρ= density
W= weight of substance
V= volume of substance

Fig 2. Pycnometer method

36
 1- pyknometer - capacity 2-10ml , conforming to the dimension
given in fig. 1
2- Constant temp. bath – water bath having a depth of at least 300mm,

capable of being maintained with in 0.05Co of desired temp.

3- bath thermometer
4- pyknometer holder .

Calibration process of (Electrical Balance (2-digit))

Origin: China
1- Run the electric balance for 5 seconds for the purpose of stabilizing the
device
2- push (cal.) button
3- Carefully place the standard test sample, which weighs 200 g, on the
center of the weighing plate.
4- We notice (Cal.) in the balance screen that includes the option of
modification
5- After that (unload) appears on the screen, which means modification is
done.
6- We raise the standard test weight and the scale returns to the weight mode.

Calculation and results

- Repeat the above test by using different petroleum
products and record the results.
- Calculate the specific weight for the petroleum products
- Calculate the standard density (API) for crude oil or oil
products by using this equation:

specific Gravity= density of substance/ density of water

141. 5
𝐴𝑃𝐼 = − 131.5
specific Gravity

37
 Discussion:
- Which method is more accurate?
- What is the important variable that the density is
depends on?...Explain
- What is the advantage of (API)?

References:
1- Viana M, Jouannin P, Pontier C, Chulia D. About pycnometric density
measurements. Talanta. 2002 May 24;57(3):583-93.
2- Zhou, Z., Ren, T., Li, M., He, M. and Zhou, X., 2023, February. Study on
Temperature Measurement of Petroleum Product Density Analyzer Based on
Hydrometer Method. In Journal of Physics: Conference Series (Vol. 2428,
No. 1, p. 012001). IOP Publishing.
3- van den Berg, L., Pronk, M., van Loosdrecht, M.C. and de Kreuk, M.K., 2023.
Density measurements of aerobic granular sludge. Environmental T

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