2018-

2019

Duhok polytechnic university

Technical college of engineering

Petrochemical department

COURS Pollution Control (practical)

:

Lecturer: Mr. Ahmad

Abdulstar
Teaching
Assistant
:Mrs.

Name of
:.exp

��� for Fractional Distillation of Crude

Petroleum

Submitted Ìbrahím Dêwalí

��:
3/30/2019

Experiment ❸
No:

Date : March 30,

2019

1
 Aim or
Objective:
In this experiment, we'll be studying how different environmental factors, such as
the number of trees or cars, affect air pollution. and explain why certain areas have
more air pollution than others, and determined contaminated in air by Atomic
Absorption Spectrophotometer AA-7000

. Introducti
on:
Air pollution is the introduction of chemicals, particulate matter, or biological
materials that cause harm or discomfort to humans or other living organisms, or
damages the natural environment, into the atmosphere. The atmosphere is a
complex, dynamic natural gaseous system that is essential to support life on planet
Earth. Stratospheric ozone depletion due to air pollution has long been recognized
as a threat to human health as well as to the Earth's ecosystems. An air pollutant is
known as a substance in the air that can cause harm to humans and the
environment. Pollutants can be in the form of solid particles, liquid droplets, or
gases. In addition, they may be natural or man-made.

Atomic Absorption Spectrophotometer AA-7000

:
Fractional distillation is the most common form of separation technology used
in petroleum refineries, petrochemical and chemical plants, natural gas
processing and cryogenic air separation plants. In most cases, the distillation is
operated at a continuous steady state. New feed is always being added to the
distillation column and products are always being removed. Unless the process is
disturbed due to changes in feed, heat, ambient temperature, or condensing, the
amount of feed being added and the amount of product being removed are
normally equal. This is known as continuous, steady-state fractional distillation
.Industrial distillation is typically performed in large, vertical cylindrical columns
known as "distillation or fractionation towers" or "distillation columns" The
distillation towers have liquid outlets at intervals up the column which allow for
the withdrawal of different fractions or products having different boiling points or
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boiling ranges. By increasing the temperature of the product inside the columns,
the different hydrocarbons are separated. The "lightest" products (those with the

2
lowest boiling point) exit from the top of the columns and the "heaviest" products
(those with the highest boiling point) exit from the bottom of the column.
For example, fractional distillation is used in oil refineries to separate crude oil into
useful substances (or fractions) having different hydrocarbons of different boiling
points. The crude oil fractions with higher boiling points:

 have more carbon atoms

 have higher molecular weights

 are less branched chain alkanes

 are darker in color

 are more viscous

 are more difficult to ignite and to burn

The diagram below summarises the main fractions from crude oil and their uses,
and the trends in properties. Note that the gases leave at the top of the column,
the liquids condense in the middle and the solids stay at the bottom.
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Fig -1 the fractionating column

3
As you go up the fractionating column, the hydrocarbons have:

❶ lower boiling points

❷ lower viscosity (they flow more easily)

❸ higher flammability (they ignite more easily).

Table (1) The fractions:

Laboratory
Distillation:
The complex mixture of hydrocarbons in crude oil can be separated
into fractions by the technique of fractional distillation. The laboratory
demonstration of the fractional distillation is illustrated on the right diagram. A
simulated synthetic crude oil is used for health and safety reasons. As the crude oil
vapour ascends the fractionating column the highest boiling liquid hydrocarbons
condense out and the lowest boiling hydrocarbon liquid's vapour exits the top of
the fractionating column and enters the condenser and runs into the collection tube.
In this way you can distil over progressively higher boiling fractions, which are
themselves narrow boiling point ranges of different hydrocarbons of similar carbon
chain length e.g. C6 to C8 etc.
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4
 Fig 2 (laboratory fractional distillation)

Apparatus and materials:

❶ distillation flask – flask with a side arm shall be of size that

is at least 50% larger than the volume of charge
❷ capacitor pass through the cooling bath
❸ magnetic stirring bar , boiling chips can be used as
alternative
❹ an electric heating mantle covering the lower half of the
flask
❺ thermometer
❻ graduated cylinder to receive the distillate
❼ a sample of crude oil
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Fig 3 (lab oratory fractional distillation)

5
 Procedure:

❶ Place 100 ml of sample in the distillation flask.

❷ Place few pieces of crushed glass on the bottom of the flask control boiling
process.

❸ Gradually raise the temperature observe rising vapors and then record the
amount of distillate at the corresponding temperatures.
❹ Determine the proportion of distillates and specific gravity and API gravity
versus boiling points.
❺ When you reach the boiling point to 350c stop distillation process and transfer
residue to another device where complemented by fractional distillation under
reduced pressure less than 40 mm hg.
❻ Report the color of each fraction.

Results and calculation:

Table 2: Temperature for volume of distilled of petroleum oil distillation

according to ASTM method
Volume (ml) Temperature oc Temperature F
%
st
1 drop 56 132.8
(IBP)
3 60 140
6 93 199.4
9 105 221
12 116 240.8
15 120 248
18 130 266
21 140 284
24 150 302
27 156 312.8
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30 170 338
33(FBP) 176 348.8 Record :

6
Volume distilled : 31.35/33 ml
Volume of residue : 0.891/33 ml
Volume of recovery : 32.241/33ml
Volume of total loss : 0.759/33 ml
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7
 Y=150 -120

X=24 -15

∆Y
Slop= ∆ X

150−120
Slop= 24−15
=3.3

200

180

160

140
Temperature, 0C

120

100

80

60

40

20

0
0 5 10 15 20 25 30 35

Volume%

Volume of distilled (%) against temperature

(°C)
Figure 4: Volume of distilled against temperature of petroleum
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Table 3: Mass and Volume of cylinder of product

8
N Mass Tutorial
of Mass of: Volume Mass of Density
cylinder cylinder (mL) Product (g/ml) S.G API.G
o Empty Full(g)
(g) ❶
❶ 31.88 39.28 10 7.4 0.74 0.74 59.72
❷ 32.01 39.46 10 7.45 0.745 0.745 58.43
❸ 26.38 30.69 5 4.31 0.431 0.431 196.81
❹ 29.68 38.18 10 8.5 0.85 0.85 34.97
Measure the percentage recovery (sample being distilled) in the measuring
cylinder.
31.35 from 33 ml
❷ Measure the percentage residue.
0.891 from 33 ml
❸Calculate the total percentage recovery and total percentage loss.
Volume of total recovery = volume of residue + volume of distilled
= 0.891 ml + 31.35 ml
= 32.241 ml from 33 ml
Volume of total loss = 33 ml – volume of total recovery
= 33 ml – 32.241 ml
= 0.759 ml from 33 ml

Discussi
on:

This type of experiment is useful to saw the cuts of crude oil

directly .. in the first time when we make the experiment we
didn’t get the current result because before we do the experiment
we add a solvent (xylene) to the crude oil the solvent decreased
the viscosity of the crude so after heating the crude all the crude
evaporated and we didn’t get the cuts …so we did the experiment
for second time but we didn’t add solvent (xylene) to our sample
3/30/2019

so we get the accurate result,, The property of hydrocarbons that lets

fractional distillation to work is the Boiling point,,the fraction with the lowest
boiling point leave the column from the top,,As hydrocarbon increase in chains

9
inter molecular force increase so the boiling point increases and become harder to
be separated.

❶ What information does the boiling range give on the composition the properties
of the crude oil?

���-Degree API gravity decrease, with the increase of mid percent boiling
point temperature of the narrow fractions, because the value of API is inversely
related to specific gravity As shown at the figure below , the API gravity decrease
-with the increase the temperature, this relation can explain all the change in
petroleum products composition with the change of boiling point, if the boiling
point increase the API gravity decrease resulting in heavy crude oil contain much
hydrocarbons with aromatic hydrocarbons , this crude oil will contain less gasoline
and will not be commercial , and if the boiling point decrease it will make the
inverse. If the boiling range of petroleum products were low , the petroleum
products will be Volatile and easy to evaporate that’s make the storage and
transferring of such products is dangerous , also in our life if boiling range of some
petroleum products were low it will evaporate quickly make a toxic gases that we
can breathing them causing problems. Also when the boiling ranges are high it will
effect at the Efficiency of them and the ability to burn inside the engines.

❷ How can distillation characteristics of hydrocarbon affects their safety and

performance?
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���-when the petroleum products are distillated , the different hydrocarbons
compounds inside the petroleum products will separate that cause decreasing in
boiling point of the distillated fraction making it easy to evaporate and explosive

❸ What is the major determinant of the tendency of a hydrocarbon mixture to

produce potentially explosive vapour ?

���-the major determinant of the tendency of a hydrocarbon mixture to

produce potentially explosive is the boiling range of the hydrocarbons inside the
mixture, if the boiling range is low the mixture is more able to explosive , gas most
easy to ignite and control less so for petrol/diesel and coal the most difficult to ignite
and control.

❹ What is the factor affecting the accuracy of the results?

���-There many factors affecting on the accuracy of this experiment , first the
loses of vapor from the flask and all joints of the instrument when it evaporate , if
the flask hole around the thermometer was not closed completely, and also the
temperature effect the results because we shouldn’t heat the sample rapidly it will
evaporate more than one component so the result will not be accurate .

Conclusion:

From this experiment of oil distillation according to ASTM method by using

petroleum as the sample, it can be concluded that the temperature is the main factor
of vaporization of the fuel which means that the fuel will be easier to vaporize due
to the increasing temperature due to high volatility in the fuel that can easily form a
flammable mixture. Based on Figure 4, the first drop was produced at 56˚C (initial
boiling point) and final boiling point of 176˚C was obtained at (31.35 mL from 33
ml) of final volume of distilled where the increased the temperature, the higher the
volume of petrol distilled and vaporize, the longer the time taken for the petrol to
reach the final boiling point from starting of the first drop compared to a low
3/30/2019

temperature. Based on Table 2, the percentage of oil distilled is (31.35 mL from 33

ml) and the percentage of residual is (0.891 mL from 33 ml) which means the total

11
recovery of gasoline obtained was (32.241 mL from 33 ml) where the higher of
distilled amount was produced by increasing the temperature. For a given
temperature, as the temperature increase it makes the fuel more easily to vaporize
as this fuel has a high volatility. This means that a highly volatile fuel is more
likely to form a flammable or explosive mixture with air than a low volatile fuel.
The percentage of recovery is high because it contains various fraction of
petroleum sample where in this experiment, the light distillate is produce at the
temperature range of 56˚C- 82.1˚C (naphtha, gasoline) and the middle distillate at
the range of 96.3˚C-176˚C (kerosene, diesel oil). At the residual percentage
consists of moisture contain. Lastly, there is percentage of the light vapors that
vaporize to the surrounding during condensation time that make the percentage of
the recovery and residual cannot achieve 100% distillation.

Recommendations:

As the recommendations, in order to overcome possible errors and also to obtain

more accurate and desirable data of results of this experiment in the future, it is
necessary to clean up the apparatus first before using it to ensure the apparatus is
contamination-free. The sample that will be used for the experiment which is
petroleum must be new petroleum sample (avoid using the recycle petroleum from
previous experiment to conduct the same experiment in future to avoid the
decrease in quality of petroleum). Next, while pouring 32 ml of petroleum, it is
necessary to be more careful and ensure there is no spillage during pouring which
can also affect the results that will be obtained. Then, in order to avoid parallax
error that caused an error to the experiment, during observing and reading the
values of volume of distilled and temperature of boiling point starting from initial
boiling point (first drop) to final boiling point (final volume of distilled), it is
necessary for the position of eyes must be in the same level and parallel as the
meniscus of the measuring cylinder and thermometer, respectively, which results in
boiling point temperature and time taken obtained will be more accurate as boiling
point temperature and time must to be recorded for specified volume of distilled.
3/30/2019

Reference:
s

12
➲ https://en.wikipedia.org/wiki/Fractional_distillation
➲ http://energyeducation.ca/encyclopedia/Fractional_distillation
➲ https://www.bbc.com/education/guides/zyvc6fr/revision/1
➲http://www.bbc.co.uk/schools/gcsebitesize/science/aqa_pre_2011/rocks/fuelsrev
7.shtml
➲ https://www.patana.ac.th/parents/curriculum/chemistry/units/LR1202.html
➲ http://www.docbrown.info/page04/OilProducts02.htm
➲ https://owlcation.com/stem/making-crude-oil-useful-fractional-distillation-and-

�.�
cracking

Table : Temperature for volume of distilled of petroleum oil distillation

according to ASTM method.
Volume (ml) Temperature oc
%
st
1 drop 54
(IBP)
5 59
10 65
20 74
30 83.5
40 94.5
50 104.5
60 114
70 125.5
80 141.5
90 173
95 178
3/30/2019

(FBP) 180

13
TUTORIAL:
❶Measure the percentage recovery (sample being distilled) in the measuring
cylinder.
96 %
❷Measure the percentage residue.
2%
❸Calculate the total percentage recovery and total percentage loss.
Volume of total recovery = volume of residue + volume of distilled
= 2 ml + 96 ml = 98 ml
Percentage recovery = (98 ml / 100 ml) x 100%
= 98 %
Volume of total loss = 100 ml – volume of total recovery
= 100 ml – 98 ml
= 2 ml
Percentage loss = (2 ml / 100 ml) x 100
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14
 Y=141.5 - 94.5

X=80 - 40
∆Y
Slop ¿
∆X

141.5−94.5
Slop ¿ =1.175
80−40

200

180

160

140
Temperature

120

100

80

60

40

20

0
0 20 40 60 80 100 120

Volume%
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= 2%

Record:

15
Volume distilled : 96 ml
Volume of residue : 2 ml
Volume of recovery : 98 ml
Volume of total loss : 2 ml
3/30/2019

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