OFFICIAL REPORT PRACTICUM OF CHEMICAL SEPARATION
PRINCIPLES
FRACSINATION DESTILATION
CHAPTER 1
INTRODUCTION
1.1 Background
Separation method is a method used to separate or purify a compound that has a
related chemical composition from a material, on a laboratory scale or on an
industrial scale. One method of separation is distillation. Distillation or distillation is
a method of separating liquids from their mixtures based on differences in boiling
points or the ease of evaporation (volatility) of a substance (Wonorahardjo &
Surjani, 2013). The working principle of distillation is that heating occurs and one of
the components of the mixture will evaporate after reaching its boiling point. The
vapor that is formed will enter the condenser pipe where there will be a cooling
process so that droplets will form that fall into the Erlenmeyer, commonly called a
distillate.
In Indonesia, which is an oil-producing country in the world, which in
processing crude oil or crude oil into finished oil, it must go through several stages
including using the fractional distillation method. Fractional distillation or multilevel
distillation is a process of purification of liquid substances or compounds in which
the mixing substance is a liquid compound that has a low boiling point and does not
differ much from the boiling point of the compound to be purified. In this
distillation, a multilevel column (fractionation) is used on each plate with the aim of
purifying the distillate underneath. The higher you go, the less volatile the liquid is.
Therefore,
1.2 Formulation of the problem
1.2.1 What is the refractive index of the resulting distillate?
1.2.2 What is the percentage purity of each distillate (methanol)?
1.3 Aim
1.3.1 Determining the refractive index of the distillate
1.3.2 Determining the percentage of distillate purity
CHAPTER II
LITERATURE REVIEW
2.1 Distillation
Distillation is a method of separating liquid substances from a mixture based on
differences in boiling points. In a simple distillation process, a mixture can be
separated if the constituent substances have a high enough difference in boiling
points. For example, in the separation of sodium chloride and water from a NaCl
solution, the solvent which has a low boiling point in this case water is evaporated
and then condensed (condensed) again to get pure water (aquades). If this process is
continued, all the water will evaporate and condense so that only solid sodium
chloride is left behind (Yazid, 2005).
Base The difference from separation by distillation is that if a mixture of its
components is evaporated, the composition of the vapor phase will be different from
that of the liquid phase. Components that have a lower boiling point will get a
composition that tends to be larger in the vapor phase, this steam will later be
condensed and boiled again in stages, a purer composition will be obtained in one of
the components (Abbasato, 2007).
2.2Fractionation Distillation
Fractional distillation or multilevel distillation is the process of separating the
distillation into parts with a higher boiling point which further separates these parts
for re-distillation. Fractional distillation is a process of purification of liquid
substances/compounds where the mixing substance is a liquid compound that has a
low boiling point and does not differ much from the boiling point of the compound
to be purified. Or it can be said, fractional distillation aims to separate compounds
from a mixture whose components have relatively small differences in boiling
points. An example of this distillation application is usually used to separate
mixtures of acetone- methanol, carbon tetrachloride-toluene, and so on.
The purpose of using this fractionation column is to separate the vapors of a
mixture of liquid compounds whose boiling points are almost the same or not much
different. Cause and effect there is a barrier in the fractionation column causing
vapors
that have the same boiling point to vaporize together or compounds that have low
boiling points will continue to rise until they finally condense and fall as distillates,
while compounds with higher boiling points, if they have not reached their boiling
point, then the compound will drip back into the distillation flask, finally heating
continues until it reaches its boiling point. The compound will evaporate, condense,
and fall or drip as a distillate.
Fractional distillation is used for components that have close boiling points.
Basically the same as simple distillation, only fractional distillation has more
condensers so that it is able to separate two components that have different boiling
points that are close together. In this distillation, a purer chemical substance will be
obtained because it passes through many condensers (Anonime, 2012).
Figure 1. Fractionation Distillation Equipment Circuit
2.3 Refractive Index and Distillate Purity Percentage
A common way used to describe distillation results is to draw a distillation
curve, where the composition, boiling point or other physical properties of the
distillate are expressed in terms of the percent or amount of distillate. The resulting
distillate can be searched for its refractive index with a refractometer. The figure
below depicts a solution undergoing fractional distillation.
Figure 2. The solution undergoes fractional distillation
To determine the purity of the distillate, it can be done by comparing the
refractive index of the distillate obtained from measurements with a refractometer.
After that, the refractive index is tested so that the percentage of purity can be
obtained.
Method calculate the % purity of the distillate:
� ���𝒑𝒆�−� �����
x (% upper limit - % lower limit) + % lower limit
��𝒘�𝒉
� �����
���������−�
��𝒘�𝒉
Information :
n = refractive index
n upper limit, final limit = refractive index of methanol with a range that is not too
far from the refractive index of methanol.
2.4 Working Principle of Fractionation Distillation
2.4.1 Scale Laboratory
In principle, fractional distillation is the same as simple distillation, the
difference is in the difference in boiling points between components, where for
simple distillation the difference in boiling point is greater than 30℃, while
fractional distillation the difference in boiling point is <30℃, this situation is
because in multilevel distillation there is a fractionation column. .
Column The long distillation of the distillation apparatus used in the laboratory
provides a large surface area for the rising vapor and descending liquid to come into
contact. At the top of the column, a thermometer is used to measure the temperature
of the first fraction rich in the more volatile A component. As the distillation
progresses, the scale of the thermometer increases indicating that the less volatile
component B is also carried away. The receiving container must be changed at
certain intervals.
If The difference between the boiling points of A and B is small, fractional
distillation must be repeated to obtain a better separation. An example of fractional
distillation is in the production of petroleum which takes place on a very large scale
(Reski, 2012).
Figure 3. Fractionation Distillation
2.4.2 Industrial Scale
First, crude oil is distilled under atmospheric pressure and then under vacuum.
When using atmospheric pressure, petroleum is heated at a temperature of no more
than 370℃ because higher temperatures will cause cracking or decomposition of
hydrocarbons. This should be avoided because the quality of the saturated
hydrocarbons formed will decrease. Distillation at atmospheric pressure will produce
a fraction with a boiling point of about 30℃ to 350℃-360℃. This fraction consists
of compounds that are useful for humans, namely gasoline, kerosene, diesel oil
(diesel), and jet fuel (aftur). In addition, it also produces raw materials for
petrochemical synthesis such as benzene, ethylbenzene, xylene, ethylene, propylene,
and butadiene (Anonime, 2014).
Figure 4. Schematic of petroleum fractionation
CHAPTER III
RESEARCH METHODOLOGY
3.1 Tools
• Distillation Pumpkin
• Fractionation Column
• Condenser
• Test tube
• Thermometer
• Hose
• Stative
• Clamp
• 100 ml beaker
• Measuring Cup 10 ml
• refractometer
• Drop pipette
3.2 Material
• Spirit
• Aquades
• Methanol 50%
• Methanol 60%
• Methanol 70%
• Methanol 80%
• Methanol 95%
3.3 Experimental Procedure (in the form of a flow chart)
100 mL spiritus
- Stuffed into distillation squash
- Heated to 64.5 ℃
- Wait until the destilat comes out
Destilat
- Every 10 mL of destilat that comes out, accommodated
into a measuring glass
- Measuring the refractive index using a refractometer
destil at bias index
- comparing the destilat bias index with the methanol
bias index 95%, 80%, 70%, 60%, dan 50%
- calculating % purity of destilat
percent purity of
CHAPTER IV
RESULTS AND OBSERVERS
4.1 Observation Results
The results of observation
No. Procedure of Experiments Suspect/Reaction Conclusion
Before After
➢ Empy Distillaion ➢The distillation CH3OH(aq) -> CH3OH(l) ➢ Refractive index of
100 mL Denaturated Alcohol Flask flask is filled with distillate = 1,330102
- Filled into the distillation flask. ➢ The temperature
100 mL of spirits ➢ Refractive index of
- Heated up to 64.5⸰C. of Denatured
- Wait until the distillate comes out. alcohol 25⸰C ➢The temperature methanol 95% =
Distillate ➢ The Denaured of Denatured 1,330202
Alcohol ➢ Refractive index of
- Every 10 mL of the distillate that comes alcohol 64,5⸰C
out, is accommodated into a beaker evaporates in the
➢ The distillate out methanol 80% =
glass. fractionating
- Measure the refractive index using a column and then ➢The distillate 1,330200
refractometer. flows in the drips and then it ➢Refractive index of
Distillate refractive index condenser is accommodated methanol 70% =
➢ The distillate
- Compare the refractive index of the in a measuring 1,330101
flows in the
distillate with the refractive index of ➢Refractive index of
condenser cup as much as
methanol 90%, 80%, 70%, 60%, 50%.
➢ Refractive index methanol 60% =
- Calculate %purity of the distillate. 10 mL
of distillate: 1,320202
Percent purity of
1,330102
➢ Refractive index ➢%purity of ➢Refractive index of
of methanol 95% distillate = 70% methanol 50% =
= 1,330202 1,320201
➢ Refractive index ➢ Percent Purity of the
of methanol 80% distillate = 70%
= 1,330200
➢ Refractive index
of methanol 70%
= 1,330101
➢ Refractive index
of methanol 60%
= 1,320202
➢ Refractive index
of methanol 50%
= 1,320201
4.2 Analysis and Discussion
Distillation is a method of separating liquid substances from a mixture based
on differences in boiling points. In a simple distillation process, a mixture can
be separated if the constituent substances have a high enough difference in
boiling points. For example, in the separation of sodium chloride and water
from NaCl solution, the solvent which has a low boiling point in this case the
water is evaporated and then condensed (condensed) again to get pure water
(aquades). If this process is continued, all the water will evaporate and
condense so that only solid sodium chloride is left behind (Yazid, 2005).This
distillation aims to separate compounds from a mixture whose components
have relatively small differences in boiling points (Dzikrullah, 2016).
Distillation works on the basic principle of pevaporation of a liquid by
heating and then condensing the vapor back into a liquid, which is called a
distillate. This distillation is a method of separating Raoult's Law based on
differences in boiling points. Raoult's law is used to explain the phenomenon
that occurs in the separation process using the distillation method explaining
that the vapor pressure of a component that evaporates in a solution is equal
to the vapor pressure of the pure component multiplied by the fraction of the
component that evaporates in solution at the same temperature.
This fractional distillation practicum aims to: Knowing the results of the
refractive index of each methanol solution (distillate) and the percentage of
purity of the methanol solution (distillate). This practicum begins by inserting
100 mL of spirit into a distillation flask and then heating it to a temperature
of
64.50C. This is because the distillate to be obtained (methanol) has a boiling
point of 650C so that the temperature is kept constant to prevent the entry of
ethanol into the distillate and a high-purity distillate is obtained.
When the temperature has reached 64.50C the distillate begins to be
produced. When it reaches the boiling point, the spirit will become vapor and
pass through a zigzag-shaped fractional column. Then the steam will be
cooled with circulating water so that the water can fill all parts of the
condenser so that a perfect cooling process is produced. The presence of a
cooler indicates a condensation event so that the water vapor will turn back
into a liquid which
is accommodated in a measuring cup. The thermometer at the top of the
column serves to measure the first fraction, namely spirit, and to keep the
temperature constant.
The next step is to accommodate every 10 mL of distillate that comes out
into the measuring cup. Then each measuring cup containing the distillate
was measured byJust use a refractometer to find out the index of refraction.
After measuring with a refractometer, the refractive index of the
distillate is
1.330102.
The next step is to measure the purity of the distillate obtained by
comparing it with the refractive index of methanol.
Table 4.2.1 Refractive index of methanol at various percentages
No Methanol Percentage Refractive Index
1 95% 1.330202
2 80% 1.330200
3 70% 1.330101
4 60% 1.320202
5 50% 1.320201
Because the refractive index of the distillate is 1.330102, 80% methanol with
an index of 1.330200 is used as the upper limit and 70% methanol with an
index of 1.330101 as the lower limit. By plugging these numbers into the
formula, the distillate purity is 70%. This shows that the purity of methanol is
70% and the remaining 30% is other components.
CHAPTER V
CONCLUSIONS AND SUGGESTIONS
5.1 Conclusion
Based on the results of the practicum and analysis above, it is obtained:
1. Refractive index of distillate = 1.330102
Refractive index of methanol 95% = 1.330202
Refractive index of methanol 80% = 1.330200
Refractive index of methanol 70% = 1.330101
Refractive index of methanol 60% = 1.30202
Refractive index of methanol 50% = 1.320201
2. Based on calculations using the formula, obtained a distillate purity of 70%
which indicates that the purity of methanol is 70%.
5.2 Suggestions
When calculating the percent purity of the distillate, it is hoped that you
will be more careful in determining the upper and lower limits according to
the distillate value obtained. As well as for the next practicum, it is expected
that the practitioner before doing the practicum understands the flow of the
stages and is careful and thorough when the practicum takes place.
Answer the question
1. Explain the principle of fractional distillation.
Answer:
The basic principle of distillation is the evaporation of a liquid by heating and
then condensing the vapor back into a liquid, which is called a distillate.
Distillation is a method of separating Raoult's Law based on differences in
boiling points. Raoult's law is used to explain the phenomena that occur in
the separation process using the distillation method explaining that the vapor
pressure of a component that evaporates in solution is equal to the vapor
pressure of the pure component multiplied by the fraction of the component
that evaporates in solution at the same temperature.
2. How to overcome over heating in the distillation process? Explain!
Answer:
The way that can be done to overcome over heating in the distillation process
is to use a boiling stone so that the heat can be evenly distributed in all parts
of the mixture, because an even temperature can prevent overheating. In
addition, the prevention of overheating can be done also by calculating the
time and evaporation and using a thermometer to monitor the temperature of
the distillate. If the temperature has reached a predetermined limit, then the
heating device can be turned off.
3. What can be done so that the distillation can run smoothly? Explain!
Answer:
The way that can be done so that the distillation can run smoothly is to find
and understand the distillation reference material properly, prepare the tools
and materials needed in the distillation experiment correctly and completely,
understand the steps of the distillation experiment and how to properly
assemble the distillation apparatus and treat it. Experiment carefully and
responsibly.
REFERENCES
Abbasato, Tony Irwanto and Eko Aris Budiarto. 2007. Efficiency of Sieve Tray
Column in Distillation Containing Three Components (Acetone-Alcohol-
Water). Technoin National Seminar
Azizah, Utiya, et al. 2009. Practical Guide to Analytical Chemistry II. Surabaya:
Department of Chemistry Unesa.
Pecsok, Robert L, etc. 1976. Modern Methods of Chemical Analysis Second
Edition. New York: John Wiley & Sons Publisher.
Poedjiastuti, Sri, et al. 2014. Practical Guide to Analytical Chemistry II:
Fundamentals of Chemical Separation. Surabaya : Department of Chemistry,
FMIPA Unesa
Yazid, Estien. 2005. Physical Chemistry For Paramedics. Yogyakarta : Andi.
ATTACHMENT
1. Picture Documentation
PICTURE DESCRIPTION
Pengukuran volume spirtus
100mL
Memasukkan batu didih ke labu
destilasi
Memasukkan 100 mL spirtus
yang sudah diukur ke dalam
labu destilasi
Rangkaian alat destilasi
Pengambilan methanol
menggunakan pipet volume
untuk dilakukan pengenceran
Memasukkan methanol ke
dalam labu ukur
Mengocok methanol yang sudah
ditambahkan dengan aquades
sampai tercampur
Memasukkan methanol yang
telah di encerkan ke dalam gelas
kimia
Menutup methanol di dalam
gelas kimia dengan plastik wrap
Methanol 50%, 60%, 70%, 80%,
dan 95%
Proses destilat yang keluar dan
ditampung di gelas kimia
Alat refractometer untuk
mengukur indeks bias destilat
2. Perhitungan
