CPB30503- Petrochemicals & Petroleum Refining Technology

Experiment 5: Oil Distillation According to ASTM Method P a g e |1

1.0 OBJECTIVES

i. To determine the percentage of distilled amount against temperature of petroleum

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

2.0 SUMMARY

This experiment has been carried out in order for the student to study about the
oil distillation according to ASTM method. From this experiment the objectives that
have been highlighted are determination of the percentage of distilled amount against
temperature of petroleum product sample, determination of the initial and final boiling
points of petroleum sample, and lastly is the determination of the quality of various
fractions of petroleum sample. This method is widely known as it was used to
obtaining distillation data (volume % distilled versus temperature). In order for this
experiment to be ran, 100 ml of petrol need to be prepared before filled inside the
distilling flask. The temperature of the vapour when the first drop of condensate was
recorded as the initial boiling point. As 95% of the sample been distilled, the burner
flame may need to be increased and the maximum temperature was recorded as the
final boiling point. From the experiment, the percentage of oil distilled was said to be
increased with the increasing of the temperature. The result shown that, the
percentage of the oil distilled obtained was 95% with 2.7% of residual and 97.7% of
the total recovery of gasoline. The initial boiling point for the petrol was observed to
be 48C with rate of distillation average of 4.7 ml per min while the final boiling
points obtained was 187C. Based on high percentage of the recovery, it has been
identified that the fraction of petroleum can be classified into three which are light,
middle, and heavy distillates.

3.0 INTRODUCTION AND THEORY

There are three objectives that needed to be achieved from this experiment. They are
to determine the percentage of distilled amount against temperature of petroleum product
CPB30503- Petrochemicals & Petroleum Refining Technology
Experiment 5: Oil Distillation According to ASTM Method P a g e |2

sample, to determine the initial and final boiling point of petroleum sample and to determine
the quantity of various fractions of petroleum sample. In this experiment, the materials that
was used is petroleum by using the ASTM method through the Distillation Unit D86 07
model. Approximately, 100ml of petroleum was measured by using a measuring cylinder and
was poured into the cabinet compartment. A new measuring cylinder was placed at the block
support. The heater power was switched on and started with 10-20% for about 5-10 minutes
for them to start boiling.

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

After that, the percentage residue can be calculated measuring the residue left in the
flask. The total percentage recovery can be calculated by combining the percent recovery and
percent residue in the flask. The combination will be deducted by 100. Hence, the percentage
of distilled amount against temperature can be determine.

The distillations (volatility) characteristics of hydrocarbons have an important effects

on their safety and performance, especially in the case of solvents and fuels. The boiling
range will give the information on the composition, properties and behaviour of the fuel
during storage and use. Volatility is the major determinant of the tendency of a hydrocarbon
mixture to produce potentially explosive vapours. Therefore, the quantity of various fractions
in petroleum products can be determined.

OPERATING PRINCIPLE OF D86 07

D86 07 is the standard test method for distillation of petroleum products at

atmospheric pressure. The operating principle for ASTM method of D86 07 distillation unit
CPB30503- Petrochemicals & Petroleum Refining Technology
Experiment 5: Oil Distillation According to ASTM Method P a g e |3

covers the atmospheric distillation of petroleum products using a laboratory batch distillation
to determine quantitatively the boiling range characteristics of such products as light and
middle distillates. The presence of high boiling point components in these and other fuels can
significantly affect the degree of formation of solid combustion deposits. Volatility, as it
affects rate of evaporation, is an important factor in the application of many solvents

4.0 RESULTS AND DISCUSSIONS/ TUTORIAL

RESULTS
CPB30503- Petrochemicals & Petroleum Refining Technology
Experiment 5: Oil Distillation According to ASTM Method P a g e |4

Table 1: Time and temperature for volume of distilled of petroleum oil distillation
according to ASTM method

VOLUME OF DISTILLED TIME TEMPERATURE

(mL) (min) (C)
st
1 drop (IBP) 10.15 48
10 12.27 65
20 14.20 73
30 16.28 80
40 18.41 89
50 21.35 101
60 24.27 116
70 26.57 133
80 29.22 147
90 33.24 167
91 34.00 169
92 34.51 172
93 35.45 178
94 37.08 180
95 (FBP) 39.24 187

Record

Volume distilled : 95 ml

Volume of residue : 2.7 ml

Volume of recovery : 97.7 ml

Volume of total loss : 2.3 ml

CPB30503- Petrochemicals & Petroleum Refining Technology
Experiment 5: Oil Distillation According to ASTM Method P a g e |5

Volume of distilled (%) against temperature (C)

100
90 f(x) = 0.69x - 26.8
80 R = 0.98
70
60
50
Volume of distillated (mL) Linear (Volume of distillated (mL))
Volume of distilled (%) 40
30
20
10
0
50 70 90 110 130 150 170 190
40 60 80 100 120 140 160 180 200

Temperature (C)

Figure 1: Volume of distilled against temperature of petroleum

DISCUSSIONS

ASTM Distillation is the most common method for obtaining distillation data (volume
% distilled vs temperature) of gasoline, naphtha, kerosene and gas oil. In ASTM distillation,
100 ml of sample is distilled at average rate of 4.7 ml per min, the distillate is condensed. The
main purpose of this experiment is to determine the percentage of distilled amount against
temperature of petroleum product sample and to determine the initial and final boiling point
of petroleum sample. Furthermore it also to determine the quantity of various fractions of
petroleum sample. For this experiment, the sample use is petrol.

The experiment was conducted by setting the analyzer and apparatus. The result of the
experiment was obtained initially at the rate of distillation average of 4.7 ml per min and
temperature at 48C, which is the initial boiling point. This experiment continued untiled the
temperature of 89 C and the average distillation rate drop to 3.4 ml per min where the
volume distilled was 50 ml. Moreover, at the temperature 167 C the average rate of
distillation drop to 0.76 ml per min which the distilled volume was 90 ml.

The result above explained that the higher of distilled amount was produced by
increasing the temperature. For a given temperature, as the temperature increase it makes the
CPB30503- Petrochemicals & Petroleum Refining Technology
Experiment 5: Oil Distillation According to ASTM Method P a g e |6

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.

Next is about the initial and final boiling point of petroleum sample. From the result
obtained, at the temperature of 48C, 101C, and 167C, the amount distilled was 10%, 50 %
and 90% respectively. As the temperature increase, the volume of fuel take to vaporize is
much greater compare to a low temperature. The final boiling point is produce at the
temperature 187C and the value for final boiling point is 95% which was 95 ml. The total
time needed to get the final boiling point is 39.24 min.

The first recorded data have no distillation rate because at this point, the fuel start to
distilled which indicate the boiling point of petrol and did not have the range of volume to be
considered as equal comparison to calculate distillation rate. Starting, middle and end
distillation rate should be in the right proportions and distilled at the right temperatures in
order to vaporize and burn at low starting temperatures. This will result in having enough
heat to bring the combustion temperatures to a point at which the next heavier fraction will
also burn, before an excessive amount of the heavier fractions of the oil can accumulate at the
burner.

From oil distillation results, the percentage of oil distilled is 95% and the percentage
of residual is 2.7% which means the total recovery of gasoline obtained was 97.7 %. Oil
recovery is the pure oil. The percentage of recovery is high because it contains various
fraction of petroleum sample. The fraction of petroleum can be classified into three categories
which are light, middle and heavy distillates. In this experiment, the light distillate is produce
at the temperature range of 48C- 82.1C (naphtha, gasoline) and the middle distillate at the
range of 96.3C-187C (kerosene, diesel oil). At the residual percentage consists of moisture
contain. The total percentage of recovery is not equal to 100% is due to the balance of the
percentage is vaporize to the surrounding which it have owed extremely light vapors that
escaped in condensation process.
CPB30503- Petrochemicals & Petroleum Refining Technology
Experiment 5: Oil Distillation According to ASTM Method P a g e |7

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

95 %

2. Measure the percentage residue.

2.7%

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

Volume of total recovery = volume of residue + volume of distilled

= 2.7 ml + 95 ml

= 97.7 ml

Percentage recovery = (97.7 ml / 100 ml) x 100%

= 97.7%

Volume of total loss = 100 ml volume of total recovery

= 100 ml 97.7 ml

= 2.3 ml

Percentage loss = (2.3 ml / 100 ml) x 100

= 2.3%
CPB30503- Petrochemicals & Petroleum Refining Technology
Experiment 5: Oil Distillation According to ASTM Method P a g e |8

4. Plot graph volume % distilled (percentage recovery) versus temperature of distillation.

Volume of distilled (%) againts Temperature (C)

100

80

60
Volume of distilled (%)
40

20

0
40 60 80 100 120 140 160 180 200

Temperature C
CPB30503- Petrochemicals & Petroleum Refining Technology
Experiment 5: Oil Distillation According to ASTM Method P a g e |9

5.0 CONCLUSION AND RECOMMENDATIONS

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 1, the first drop was produced at 48C (initial boiling point) and
final boiling point of 187C was obtained at 95 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 temperature. Based on Table 1, the percentage of oil distilled is 95% and
the percentage of residual is 2.7% which means the total recovery of gasoline obtained was
97.7 % 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 48C- 82.1C (naphtha, gasoline) and the
middle distillate at the range of 96.3C-187C (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 100
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
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Experiment 5: Oil Distillation According to ASTM Method P a g e | 10

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.

6.0 REFERENCES
CPB30503- Petrochemicals & Petroleum Refining Technology
Experiment 5: Oil Distillation According to ASTM Method P a g e | 11

i. Yassir Ammar Ahmed. ASTM Method For Distillation Of Petroleum Products At

Atmospheric Pressure. (2014) University of Zakho, Deparment of Petroleum
Engineering.
ii. Standard Test Method For Distillation Of Petroleum Products At Atmospheric
Pressure. ASTM International D86-07. (2015).

7.0 APPENDICES