CENTRAL PHILIPPINE UNIVERSITY CHE 4203

COLLEGE OF ENGINEERING CHEMICAL ENGINEERING

BATAN, KAREN LOUISE

MAMELOCO, CYRILLE MAE
GROUP NO. 4 PATNA, NIEZA JANE Experiment No.7 Distillation
POMAR, KIM RENIER
VEDEJA, MAYRIEL ZEN

Jaro, Iloilo City, Philippines LABORATORY 1

I. Objectives

 To purify a compound by separating it from a non-volatile or less-volatile material.

 To separate a mixture of two miscible liquids (liquids that mix in all proportions) with
different boiling points.
 To determine the boiling points and other physical properties including refractive index
and density of purified materials.

II. Theory

Distillation History:
As far back as the fourth century
B.C. Aristotle suggested the possibility of
spirit distillation when he wrote: "Seawater
can be made potable by distillation as well
and wine and other liquids can be
submitted to the same process." It is an
age-old process which may have begun as
early as 2000 BC. Some say that the first
use of distillation occurred in China, Egypt, or Mesopotamia for medicinal purposes as well as to
create balms, essences, and perfumes. About 1810 B.C. in Mesopotamia, the perfumery of King
Zimrilim employed this method to make hundreds of liters of balms, essences and incense from
cedar, cypress, ginger and myrth every month. These were used to embalm the dead and for
spiritual, medicinal and cosmetic purposes. Queen Cleopatra knew about distillation and is
thought to have given an account of the process in a text which is now lost. In the first century, a
Greek physician Pedanius Dioscurides made mention of this process after he noticed the
condensation on the lid of a vessel in which some mercury was being heated.
Historians state the alembic was probably invented around AD 200 - 300 by Maria the
Jewess, or Zósimo of Panoplies an Egyptian alchemist and his sister Theosebeia, who invented
many types of stills and reflux condensers. Others state that during the eighth or ninth century
Arab alchemists devised the alembic in an effort to obtain finer essences for perfumes while
other Arab alchemists used the alembic in an effort to convert base metal into gold. "Ambix" is a
Greek word defined as a vase with a small opening. The vase was part of the distillation
equipment. Initially, the Arabs changed the word "Ambix" to "Ambic" and named the distillation
equipment "Al Ambic". This was later changed to alembic in Europe.

Definition:
Distillation is the process of heating a liquid solution, or a liquid-vapor mixture, to derive off a
vapor and then collecting and condensing this vapor. In the simplest case, the products of a
distillation process are limited to an overhead distillate and a bottoms, whose compositions differ
from that of the feed. Distillation is one of the oldest and most common method for chemical
separation. Historically one of the most known application is the production of spirits from wine.
Today many industries use distillation for separation within many categories of products:
petroleum refining, petrochemicals, natural gas processing and, of course, beverages are just
some examples. The purpose is typically the removal of a light component from a mixture of
heavy components, or the other way around, the separation of a heavy product from a mixture of
light components.
Role of Raoult’s Law and Dalton’s Law
The temperature at which the vapor pressure of a liquid becomes equal to the pressure of
the surrounding area is known as the boiling point of that liquid. At this temperature point, the
liquid is converted into its vapor form via the formation of vapor bubbles at its bulk.
For a mixture of liquids, the distillation process is dependent on Dalton’s
law and Raoult’s law. As per Raoult’s law, the partial pressure of a single liquid component in an
ideal liquid mixture equals the product of the vapor pressure of the pure component and its mole
fraction. According to Dalton’s law of partial pressures, the total pressure exerted by a mixture of
gases is equal to the sum of the partial pressures of all the constituent gases.
When a mixture of liquids is heated, the vapor pressure of the individual components increases,
which in turn increases the total vapor pressure. Therefore, the mixture cannot have multiple
boiling points at a given composition and pressure.
The K-value for a component i is defined as: Ki=yi/xi
The K-value is sometimes called the equilibrium “constant”, but this is misleading as it
depends strongly on temperature and pressure (or composition). The relative volatility between
components i and j is defined as:

ij = = Ki/Kj

Types of Distillation
Some important types of distillation include:
 1. Simple distillation- Simple distillation involves heating the liquid mixture to the boiling
point and immediately condensing the resulting vapors.
2. Fractional distillation- Fractional distillation is often used to separate mixtures of liquids
that have similar boiling points. It involves several vaporization-condensation steps
Date Performed: September
(which takes 6, 2019
place in a fractioning column). Teacher:
Date3.Submitted:
Steam distillation- Steam
September 13, 2019distillation is oftenEngr.
used Sharon
to separate
Rose heat-sensitive
Dumam-ag components
in a mixture.
4. Vacuum distillation- This is ideal for separating mixtures of liquids with very high
boiling points.
5. Air-sensitive vacuum distillation-- For compounds that are sensitive to air and readily
react with it, the vacuum distillation process is carried out but the vacuum must be
replaced with an inert gas once the process is complete. Such a process is often referred
to as air-sensitive vacuum distillation.
6. Short path distillation- Short path distillation is used to purify a small quantity of a
compound that is unstable at high temperatures. This is done under lowered pressure
levels and generally involves the distillate traveling a very small distance before being
collected (hence the name ‘short path’). The reduced distance traveled by the distillate in
this method also reduces the wastage along the walls of the apparatus.
7. Zone distillation- The process of zone distillation involves the partial melting of a
substance and the condensation of the resulting vapors to obtain a pure distillate. This is
carried out in a long container with the help of a zone heater.

III. Materials and Apparatus

 Materials
Ethanol
Water

 Apparatus
Iron Ring
Iron Stand
Distillation Flask
Thermometer
Stopper/Cork
Three-way Adapter
Receiving Adapter
Support Clamp
Asbestos Heating Mantle
Condenser
Cylinder
Beaker
Burner

IV. Procedure
Initially, we assembled the distillation apparatus with the help of the lab assistant who also prepared
and gave us the ethanol water mixture to be distilled. The mixture was poured into the round bottom flask
because of its volatile properties. Then, we connected the apparatus to the cooling water and the gas line.
Before proceeding with the experiment, the lab assistant gave us instructions on the range of temperatures
the data should be recorded. The rangers were 0-85ºC, 85-90 ºC, 90-95 ºC and 95-100 ºC. For the first
range of temperature, we immediately collected the distillate when the temperature reached 85 ºC. When
the temperature reached 86 ºC, we stopped collecting the distillate and measured the volume obtained
using a graduated cylinder. We repeated the procedure when the temperature reached 90 ºC, 95 ºC and
100 ºC. After the experiment, we cleaned the apparatus and returned them to the lab assistant.

V. Diagram

(see the next page for the diagram)

VI. Data and Results

Temperature, 0C Volume, ml Smell of ethanol

0 - 85 9.8 Strong
85 - 90 17.2 Mild
90 - 95 13 Weak
95 - 100 6.2 Not present

VII. Computations
Given: Required:
V1 = 9.8 ml Percent Error ( PE )
V2 = 17.2 ml
V3 = 13 ml
V4 = 6.2 ml
V0 = 50 ml
Solution:
TOTAL DISTILLATE = (V1 + V2 + V3) = 9.8 + 17.2 + 13 = 40 ml
PE = (theoretical – experimental)/theoretical = (50-40)/50
PE = 0.2 = 20%
VIII. Observation and Discussion of Result
In this experiment, four different time intervals were used for the separation of ethanol
from water. The initial volume of the mixture was 100 ml with 50 % ethanol. The first
temperature interval of heating was from 0 to 85 ͦ C and the volume of distillate was 9.8 ml. The
second interval was from 85 to 90 ͦ C, wherein the volume of distillate was 17.2 ml. Then, the
distillate was 13ml for the temperature range of 90 to 95 ͦ C and finally for the range 95 to 100 ͦ
C, the distillate was 6.2 ml.
Based from the results, it was observed that the second and the third interval had the
highest distillate collected while the last or the fourth time interval had the lowest distillate. The
total volume of the distillate was 40 ml and the last measured one was pure water so it was not
included in the computation.
The smell of ethanol was also observed in this experiment. Wherein the first one has the
strongest smell since ethanol is present in large concentration. But in the second distillate, the
smell of ethanol decreased. On the third distillate, the smell of ethanol was faint and on the
fourth measurement, the smell was completely absent as the ethanol had evaporated and pure
water remained.
The percent error was determined by getting the sum of the first three measured distillates
then the total was subtracted from the theoretical methanol content and finally dividing the whole
equation by the theoretical value which is 50. The result computed was 20% which meant there
is a 20% discrepancy from the theoretical value as compared to the experimental value.

IX. Conclusion and Recommendations

X. Applications
In the recent years, distillation makes about 95% of all current industrial separation processes. Many
of the products we use every day are the result of distillation, from the gasoline that powers our cars to the
water we drink.
One of the earliest uses of distilling was to make perfume, which began around 3500 B.C. The
aroma from various plants and herbs is contained in what are known as essential oils, which can be
extracted through distillation. Distillation has also long been used as the separation process in the
chemical and petroleum industries because of its reliability, simplicity, and low-capital cost. It is
employed to separate benzene from toluene, methanol or ethanol from water, acetone from acetic acid,
and many multicomponent mixtures. Fractionation of crude oil and the production of deuterium also rely
on distillation
Another practical use of distillation is in the laboratory. The process is used regularly in chemical
and pharmaceutical research, quality assurance testing for many consumer products and law enforcement
forensics. Distillation is used to produce a variety of alcoholic beverages, such as whiskey, rum and
brandy. Distilling the fermented material purifies and concentrates the ethanol. A variety of other
components, such as water, esters and other types of alcohol, are also collected during the distillation
process, which accounts for the unique flavor of each alcoholic spirit. Steam distillation is also used to
create natural food flavorings. The most common are citrus oils and liquid extracts of various herbs and
spices. Lastly, some people drink distilled water because they like the taste or want to avoid the minerals
found in tap water. Distilled water is commonly used in situations where the presence of minerals might
reduce the effectiveness of certain equipment, such as in steam irons or cigar humidors.

XI. References

https://byjus.com/chemistry/distillation/
https://ethz.ch/content/dam/ethz/special-interest/mavt/process-engineering/separation-processes-
laboratory-dam/documents/practica%20in%20process%20engineering%202/distillation.pdf
http://folk.ntnu.no/skoge/publications/1999/DistillationTheory/original/distillationtheory.pdf
https://www.unguentarium.eu/pages/distillation-history

XII. Documentation

Distillation Column Materials

Measurement of Distillate