CPD 20103

PETROCHEMICALS & PETROLEUM REFINING

TECHNOLOGY

OIL DISTILLATION ACCORDING TO ASTM METHOD

(LAB REPORT)

PREPARED BY:

1. NUR FARHANA BINTI ROSLIM 55102316035

2. NOR AMIRAH BINTI ROSLI 55102316012
3. NUR ANIS ALISYA BINTI MOHD FAIZAL 55102316087
4. SHARVINESWARY MUTTHUKRISHNAN 55102316032
5. DK. SOFIA BINTI AG. ABDULLAH 55101214007

LECTURER : MISS ZURAIDAH BINTI RASEP

DATE OF EXPERIMENT : 21 FEBRUARY 2018

DATE OF SUBMISSION : 28 FEBRUARY 2018

1.0 OBJECTIVES

The purpose of the experiment

 To determine the percentage of distilled amount against temperature of petroleum

product sample.
 To determine the initial and final boiling points of petroleum sample.
 To determine the quantity of various fractions of petroleum sample.

(DK Sofia)
2.0 SUMMARY

The aims of the experiment are mainly to determine the percentage of distilled amount against
temperature of petroleum product sample, to determine the initial and final boiling points of petroleum
sample, to determine the quantity of various fractions of petroleum sample has been run throughout the
experiment. The variables involve in the experiment are volume of recovery, volume of residues
(additives), initial boiling point (℃) and final boiling point (℃). after the data of results were gained,
the volume of distilled, the volume of residue (additives), initial boiling point (℃) and final boiling
point (℃) can finally be determined. The volume of distilled is 90 ml, the volume of residue (additives)
is 7.2 ml. as for the initial and final boiling points, they are 43 ℃ and 158 ℃ respectively. In relation to
the results gained, a trend graph was plotted to aid in clarification and in supporting the theory. It can
be observed on the graph generated that as the boiling point (temperature) increases, the volume of
distilled also increases. It can be concluded as a hypothesis, that the boiling point (temperature) and
volume of distilled have a directly proportional relationship. Hence, the objectives were achieved which
were to study the volume of distilled against temperature of product sample, to determine the initial and
final boiling points of petroleum sample, and to determine the quantity of various fractions of petroleum
sample has been conducted in this experiment.

(DK Sofia)
3.0 INTRODUCTION & THEORY

Basically, this experiments was about to determined the percentage of distilled amount against
temperature of petroleum product sample, determine the initial and final boiling points of petroleum
sample and to determine the quantity of various fractions of petroleum sample. The material which was
used in this experiment is gasoline by using the ASTM method through the Distillation Unit D86 07
model. For this experiment, 100mL of gasoline was measured using measuring cylinder and poured into
the cabinet compartment. Another 100mL measuring cylinder was placed at the block support to collect
the condensate gasoline. The heater power was switched on and started with 10-20% for about 5-10
minutes for the gasoline to start boiling.

Initial Boiling Point (IBP) is the first drop of the condensate liquid. The time (min) and temperature
(℃) was recorded at the first drop of the liquid. This step was repeated for every 10mL interval until
reached 90mL and after that continue with 1mL interval until the liquid stops dropping. The time taken
and the temperature was recorded. Final drop of the liquid is known as the final boiling point of the
petroleum products. So, the objective of determining the range of the boiling point was achieved.

Next, the percentage residue was calculated by measuring the remain residue in the flask. The total
percentage recovery can be calculate by combining the percent recovery and percent residue in the flask.
The combination will be deducted by 100. Thus, the percentage of distilled amount against temperature
can be determine.

The distillation’s volatility characteristics of hydrocarbons have an important effects on their safety
and performance, especially in the case of solvent and fuels. The boiling range will give the information
on the composition, properties and behaviours of the fuel during storage and use. Volatility is the major
determinant of the tendency of a hydrocarbon mixture to produce potentially explosive vapors.
Therefore, the quantity of various fractions in petroleum products can be determined.

(Sharvine)
4.0 RESULTS AND DISCUSSION/TUTORIALS

4.1 RESULTS

Initial Rate Temperature ( ˚C ) Time ( min )

First Drop 43 8.32
10 59 10.10
20 60 10.54
30 65 12.05
40 73 13.27
50 84 15.09
60 102 17.19
70 124 20.13
80 148 25.15
90 158 47.32
Table 1

Volume of distilled : 90 mL

Volume of residue : 7.2 mL

Volume of recovery : 97.2 mL

Volume of total lost : 2.8 mL

Total volume : 100 mL

180
160
140
Temperature (℃)

120
100
80
60
40
20
0
8.32 10.1 10.54 12.05 13.27 15.09 17.19 20.13 25.15 47.32
Time (minute)

FIGURE 1: Boiling point (temperature) against time (minute)

(Farhana)
 4.2 DISCUSSION

The purpose of the experiment was to determine the percentage of distilled amount against
temperature of petroleum product sample, to determine the initial and final boiling points of petroleum
sample. Furthermore, is to determine the quantity of various fractions of petroleum sample.

Based on the theory of oil distillation and producing a lot of useful products such as petrol, diesel,
bitumen and such. In this experiment, the API gravity decreases 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. Distillation characteristics of hydrocarbon affect their safety and performance
when the petroleum products are distillate, the different hydrocarbons compounds inside the petroleum
products will separate that cause decreasing in boiling point of the distillate fraction making it easy to
evaporate and explosive.

The experiment was begun by using the sample of petrol using the measurement of 100mL that
was filled in a distilling flask. Then the flask was placed inside the cabinet compartment and ensured
that the heating flask support was placed properly to avoid any hazard from occurring. After that, the
power was switched on and the control for heat was started from about 10% - 20% for about 5 – 10
minutes until the sample started to boil. Later, the measurement began to start recording when the first
drop of the distilled sample was made and later was continued from 10mL, 20mL, 30mL, 40mL, 50mL,
60mL, 70mL, 80mL and 90mL. Each of the volume was taken and the readings of time and temperature
and was observed. After the experiment, the ASTM was let cool down, before taking any measurement
of residue, recovery and distilled.

Based on the result that had been obtained, it was shown that the first drop of sample was at the
time of 8.32 at the temperature of 43 ˚C which shown the initial boiling temperature for the sample
(petrol). This is due to the characteristic of the sample which is volatile therefore making it easy to
evaporate due to the heating from the heater. After that, the reading was recorded from 10mL, 20mL,
30mL, 40mL, 50mL, 60mL, 70mL, 80mL and 90mL. The sample was distillate till the final boiling
temperature at the volume of 90mL with the time at 47.32 with temperature at 158 ˚C. From there, we
learned that the amount of time is directly proportional to the temperature and also that the time and
temperature were both affected by the numbers of hydrocarbons in the sample, the density of the sample
and also the volatile of the sample. We also can measure the final volume of the recovered petroleum
sample due to the distillation which was 97.2mL. With the amount of residue (additives) that were left
inside the flask was 7.2mL. The amount of total lost was 2.8mL. The colour of petroleum changed where
from light yellow to colourless.
 In order to support the theory, a trend graph of boiling point (temperature) vs tome (minute) was
plotted. It can be observed that as the boiling point (temperature) increases, the volume of the distilled
also increases. It can be concluded that the boiling point and the volume of distilled have a directly
proportional relationship.

There were few possible errors that occurred in this experiment. First error was heater power
were not at 20% for entire experiment. If not switch off the heater power, it could lead flask will break
down. Next, the experimenters did not listen clearly when technician was briefing the procedures in the
experiment. It could affect the result and the theory could be impossible to achieve. Last but not least,
the reading were not very accurate because of the drop of recovery oil will make the wave.

(Farhana)
 4.3 TUTORIAL
1. Measure the percentage recovery (sample being distilled) in the measuring cylinder.

Percentage recovery = (Volume of distilled / Total volume) X 100%

= (90mL / 100mL) X 100%

= 90%

2. Measure the percentage residue.

Percentage residue = (Volume of residue / Total volume) X 100%

= (7.2mL / 100mL) X 100%

= 7.2%

3. Calculate the total percentage recovery and total percentage loss.

Total percentage recovery = (Volume of recovery / Total volume) X 100%

= (97.2 mL / 100mL) X 100%

= 97.2%

Total percentage loss = (Volume of total lost / Total volume) X 100%

= (2.8mL / 100mL) X 100%

= 2.8%

(Amirah)
5.0 CONCLUSION & RECOMMENDATIONS

As a conclusion, the experiment is to distillate a sample from the crude oil using a ASTM. The
experiment was also used to determine the initial and final boiling point for the sample that was used
and also to determine the quantity of various fraction of the petroleum sample via distilled, residue and
recovery. From there, the result that were obtained were for the initial boiling temperature of 43⁰C and
the final boiling temperature was 200⁰C. Moreover, this shows that the petroleum sample (petrol) has a
high volatile level and also density. Furthermore, the amount of residue that were obtained was 2.2ml
and recovered sample was 97.2ml. From the experiment that was conducted, it can be said that the
objectives of the experiment was achieved.

As for recommendations, the experiment was needed to take a precise sample of 100ml of
petroleum sample (petrol) that was filled in a distillate flask. Other than that, the temperature of the
heater during the experiment must be increased by observing the amount of drops that was seen to avoid
from any errors from occurring during the conduction of the experiment. In addition, the readings for
the temperature must be read with the same level of the eye and the thermometer to reduce the chances
of parallax error. Lastly, the sample must be cooled down first before taking any measurement reading
to avoid any injuries from occurring.

(Anis)
6.0 REFERENCES

1. Fahim, M. A., Taher A. Alsahhaf, and Amal Sayed Elkilani. "Chapter 9." FundaGanesan, V.
(2004). Internal combustion engines (1st ed., p. 306). Boston: McGraw-Hill.mentals of
Petroleum Refining. Oxford: Elsevier, 2010. N Print
2. Flores, Ethan. Fundamentals of petroleum and petrochemical engineering. London: Auris
Reference Ltd., 2012. Print.
3. Kowalski, B, and F Mac Lennan. Process Analytical Chemistry. 1st ed. London [etc.]:
Blackie Academic and Professional, 1996. Print.
4. Ganesan, V. (2004). Internal combustion engines (1st ed., p. 306). Boston: McGraw-Hill.

(Amirah)