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1.

0 OBJECTIVES

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


product sample.
2. To determine the initial and final boiling points of petroleum sample.
3. To determine the quantity of various fractions of petroleum sample.
2.0 SUMMARY

This experiment was conducted to determine the initial and final boiling points
of petroleum sample, the percentage of distilled amount against temperature of petroleum
product sample and to determine the quantity of various fractions of petroleum sample. ASTM
Distillation is the most common method for obtaining distillation data (volume % distilled vs
temperature) of gasoline, naphtha, kerosene and gas oil. 100 ml of sample is distilled at uniform
rate of 2.079 ml per min, the distillate is condensed. The sample used was Petrol. The
experiment was conducted by setting the analyser and apparatus based on the lab manual. From
the result, the IBP (Initial Boiling Point) was obtained at 50C and at the rate of distillation
average of 4 ml per min. While the Final Drop (FBP) obtained at 173C From the data that was
obtained from the experiment, at temperature of 56C, 85.5C, and 173C, the amount of
distillation was at 10%, 50%, and 90% respectively. As the temperature increase, the amount
of distillation also increased but the time taken for each 10ml also increases overtime. The total
time taken for it to reach to the last drop was 46 minutes and 59 seconds. The first recorded
data has no distillation rate because the data was to indicate the initial boiling point of the petrol.
However, after the first recorded data, the distillation rate can be calculated using the difference
of the previous data with the current data over the time taken need for it to reach to the current
volume. From the graph, this prove that the first 12 minutes has higher rate distillation because
of the lighter fraction of the petrol are being vaporize and the rate began to slow down due to
the heavier portion of the petrol that are being vaporized. From the data obtained, the
percentage of oil distilled was 90% and the percentage of residue was 7.4% which come to
total of 97.4% of oil recovery. The percentage of recovery is high, because it contains various
fraction of the oil. From the experiment, the light distillate produces at the temperature range
of 50C until 85.5C (naphtha, gasoline) and the middle distillate is produced at the temperature
range of 101C until 173C (kerosene, diesel). From the conducted experiment, it can be
deduced that the amount of distillation increased as the temperature increased where the higher
the temperature will be easier for the sample to be vaporized. The remaining liquid residue in
the flask was due to the presence of very high boiling point compound in the sample. The
percentage of the recovery and residual cannot reach 100% distillation due to the percentage
of the light vapours that vaporized to the surrounding during condensation time.
3.0 INTRODUCTION AND THEORY

Distillation can be defined as separation of the components in a solution between liquid


and gas phase depending on their distribution. It may be carry out by two ways. Firstly, by the
production of the vapour. It can be done by boiling the liquid mixture to be separate, then any
of the vapour condense are not allowed to be return to the still, without reflux. Secondly,
returning part of the condensate back to still under some condition by intimate contact in the
condenser. There are several trays in the distillation column that allowing the travel of the gas
going up and the liquid to going down of the tray, therefore allowing both phases to mix and
thus achieve equilibrium. The feed of liquid mixture tray divides the column into a top and a
bottom section. The top known as enriching or rectification while the bottom is the stripping.
Moreover, the vapour that moves upward will exit to the top of the unit and being cool by the
condenser. That condense liquid also known as top product or distillate, are being stored in a
reflux drum, a type of holding vessel. The reflux will occur where some of the liquid is recycle
back to the column.

ASTM Distillation it the standard Test Method at atmospheric pressure for determining the
characteristic of the boiling range for petroleum products. As the working principle, it is based
on the differential or simple distillation. A batch of liquid petroleum product is charge into a
still fitted with heating device. Next, it will be boil slowly and releasing the vapour that will
rapidly withdraw into the condenser. After that, the condensate then being collect in the
receiver (ASTM DIstillation, 2012). ASTM test method covers the atmospheric distillation of
the petroleum products by batch distillation unit in laboratory. It determines the quantitatively
boiling range characteristics of such a light and middle distillate, aviation gasoline, diesel fuel,
turbine fuels, marine fuels, naphtha, kerosene, Grade 1 and 2 burner fuels and some other more.
It is designed for the analysis for distillate fuels where are not applicable to residual-containing
product in appreciable quantities. Besides, ASTM covers both of automated and manual control
instruments (Ahmed, 2014). In addition, ASTM test methods are an industry standard test for
petroleum that are widely accepted for reliability and quality (ASTM Petroleum Test Methods,
2018). There are ASTM D86 for the atmospheric distillation suitable for the low boiling
fractions and ASTM D1160 for the vacuum distillation for the high boiling fractions (Eser,
2017).
Figure 1: TBP, ASTM, EFV curves

Other than ASTM method, there are another two type of method that are commonly used
to generate laboratory data of the crude oil; True Boiling Distillation (TBP) and Equilibrium
Flash Vaporization (EFV).

As the comparison, these three methods achieving different levels of separation of


petroleum products, as related due to the different techniques used on the analysis. TBP is used
characterize the crude oil and the constitute component of crude assays. Besides, the ASTM is
used for refinery products and property calculations and others that correlations for to the
distillate fraction. While the EFV provides useful data for the flashing operations in the refinery.
Referring to Figure 1, it shows the three methods curves on 50% converged middle distillate
fraction of crude oil also showing the significant differences in IBP and EP. As the result, the
TBP is the best separation, followed by ASTM and lastly the EFV(Eser, 2017)
4.0 RESULTS AND DISCUSSION/ TUTORIAL

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

Volume of distilled (ml) Time (min) Temperature (℃)


Initial drop (IBP) 8.52 50
10 10.22 56
20 11.16 60
30 12.27 66
40 13.50 74
50 15.36 85.5
60 17.38 101
70 20.36 125
80 25.11 149
Final drop (FBP) = 90 46.59 173

Record

Volume distilled : 90 ml

Volume of residue : 7.4 ml

Volume of recovery : 97.4 ml

Volume of total loss : 2.6 ml


Volume Distilled against Temperature
120

Volume distilled (ml) 100 y = 0.6844x - 19.302


R² = 0.9124
80

60 Volume Distilled

40
Linear (Volume
20 Distilled)

0
0 50 100 150 200
Temperature (℃)

Figure 1: Volume of distilled against temperature of petroleum

DISCUSSION

ASTM Distillation is the most common method for obtaining distillation data (volume %
vs temperature) of gasoline, naphtha, kerosene and gas oil. In ASTM distillation, 100ml of
sample is distilled at average rate 2.079 ml per min, the distilled is condensed. The main
purpose of this experiment is to determine the percentage of distilled amount against
temperature of petroleum sample, initial and final boiling point of petroleum sample, and lastly
is to determine the quantity of various fractions of petroleum sample. For this experiment,
petrol was used as the sample.

The experiment was conducted by setting the analyser and apparatus. The result of the
experiment was obtained initially at the rate of distillation average of 4 ml per min and
temperature was at 50C, which is the initial boiling point. As the experiment continued, when
the temperature was at 66C, the rate of distillation drops significantly beyond this temperature.
From the plotted graph (volume distilled against temperature), the gradient of the graph will
represent the rate of distillation. The gradient of the graph begins to decrease significantly when
reaching 100C and above. This prove that a highly volatile fuel is more likely to form a
flammable or explosion mixture with air than a low volatile fuel.

Next is about the initial and final boiling point of the petrol. From the data that was
obtained from the experiment, at temperature of 56C, 85.5C, and 173C, the amount of
distillation was at 10%, 50%, and 90% respectively. As the temperature increase, the amount
of distillation also increased but the time taken for each 10ml also increases overtime. The total
time taken for it to reach to the last drop was 46 minutes and 59 seconds.

The first recorded data has no distillation rate because the data was to indicate the initial
boiling point of the petrol. However, after the first recorded data, the distillation rate can be
calculated using the difference of the previous data with the current data over the time taken
need for it to reach to the current volume. From the graph, this prove that the first 12 minutes
has higher rate distillation because of the lighter fraction of the petrol are being vaporize and
the rate began to slow down due to the heavier portion of the petrol that are being vaporized.
However, there are some residue due to its higher boiling point that cannot be reach during the
experiment makes it cannot be vaporize.

From the data obtained, the percentage of oil distilled was 90% and the percentage of
residue was 7.4% which come to total of 97.4% of oil recovery. The percentage of recovery is
high, because it contains various fraction of the oil. It can be classified as three category which
are light, middle, and heavy distillate. From the experiment, the light distillate produce at the
temperature range of 50C until 85.5C(naphtha, gasoline) and the middle distillate is produced
at the temperature range of 101C until 173C(kerosene, diesel). At the residual percentage
consists of moisture contain. The total recovery percentage cannot reach 100% because of the
extremely light vapour that has escaped the condensation process during the experiment was
being conducted.
TUTORIALS

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

= 90 %

2. Measure the percentage residue.

= 7.4%

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

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

= 7.4 ml + 90 ml

= 97.4 ml

Percentage recovery = (97.4 ml / 100 ml) x 100%

= 97.4%

Volume of total loss = 100 ml – volume of total recovery

= 100 ml – 97.4 ml

= 2.6 ml

Percentage loss = (2.6 ml / 100 ml) x 100

= 2.6%
4. Plot graph volume % distilled (percentage recovery) versus temperature of distillation

Volume Distilled (%) against


Temperature (℃)
100
173, 90
Volume distilled (ml)

80

60
Volume Distilled
40

20

0
0 50 100 150 200
Temperature (℃)
5.0 CONCLUSION AND RECOMMENDATION

From the conducted experiment, it can be deduced that the amount of distillation
increased as the temperature increased where the higher the temperature will be easier for the
sample to be vaporized. The remaining liquid residue in the flask was due to the presence of
very high boiling point compound in the sample. From Figure 1, the first drop was produced at
50 ℃ (initial boiling point) and the final boiling point of 173 ℃ obtained at 90 ml of final
volume of distilled. It is because the increased the temperature, the higher the volume of petrol
distilled and vaporized as well the longer the time taken for the petrol to reach the final boiling
point from starting of the first drop compared at a low temperature. From Table 1, the
percentage of oil distilled was 90% and the percentage of residue was 7.4% which come to
total of 97.4% of oil recovery. The percentage of recovery is high, because it contains various
fraction of the oil. It can be observed that light distillate produces at the temperature range of
50C until 85.5C (naphtha, gasoline) and the middle distillate is produced at the temperature
range of 101C until 173C (kerosene, diesel). Lastly, the percentage of the recovery and
residual cannot reach 100% distillation due to the percentage of the light vapours that vaporized
to the surrounding during condensation time.

RECOMMENDATION

There are several recommendations that need to be done when conducting the
experiment to get an accurate and precise result. Firstly, make sure not to use the recycle petrol
or sample to avoid the decrease quality of petrol used. Next, clean all the apparatus before used
to ensure that it is contamination free. Furthermore, make sure eyes are parallel and at the same
level of thermometer when taking the reading of temperature as well as the measuring cylinder
when taking the reading of volume distilled to avoid any parallax error to obtain an accurate
result. Finally, use the suitable apparatus to measure the volume of any sample to avoid error
of the reading in the future.
REFERENCES

1. Ahmed, Y. A. (2014, 11 16). ASTM method for Distillation of Petroleum Products at


atmospheric pressure. Retrieved from SlideShare:
https://www.slideshare.net/mobile/yoyoalbeatiy/astm-method-for-distillation-of-
petroleum-products-at-atmospheric-pressure

2. ASTM DIstillation. (2012). Retrieved from Sakshat Virtual Labs: iitg.vlab.co.in/?

3. ASTM Petroleum Test Methods. (2018). Retrieved from Intertek:


www.intertek.com/petroleum/astm-test-methods/

4. Eser, D. S. (2017). Petroleum Processing: Distillation Methods. Retrieved from


College of Earth and Mineral Sciences, Penn State: https://www.e-
education.psu.edu/fsc432/content/distillation-methods