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PRACTIACAL GUIDE TO DISTILLATION PRACTICES AND PRINCIPLES



The process of distillation has its origins in the 1st century AD when ancient Greek
alchemists began experimenting with the distillation of wine. Even though distillation is
commonly associated with alcohol production, the process has many other applications.
Distillation allows users to separate any mixture into its components based on the
components volatility. The process may result in nearly pure products or in some cases
partial separation of the components is desired.

INTRODUCTION

Distillation has countless applications in both laboratory and industrial settings. In


laboratory settings, researchers often run batch distillations in which a multicomponent
solution is charged into a closed vessel commonly referred to as a still. After charging the
still researchers have a plethora different laboratory scale techniques to conduct the
distillation. One technique is simple distillation, a process in which vapor flows through a
condenser producing a liquid whose concentration is dependent on Raoults Law at the
given temperature and pressure. This technique is only effective when the components
have boiling points that differ greatly.

Another technique called fractional distillation uses repeated vaporization and
condensation cycles to separate components with similar boiling points. The vapor flows
through a column packed with materials such as marbles or metal beads, as the vapor cools
and condenses on the columns walls and packing materials the liquid is reheated and the
process begins again. Each successive vaporization and condensation yields a purer solution
of the more volatile component.

Large-scale industrial applications of distillation use many of the same techniques and
principles used in laboratory settings, however the equipment looks drastically different.
Distillation columns range in size anywhere from six meters to heights greater than 90
meters. Petroleum processing is one of the most common industrial applications of
distillation. In this process distillation towers are used with multiple outlets to separate the
many components of crude oil. As the oil is heated, the vapors produced rise up the column
and a downward flowing reflux liquid cools the vapor. The vapors then condense on a
distillation plate where the desired component is collected.

Due to the broad range of applications and complexities of distillation, this publication will
only discuss the process of simple distillation. The purpose of this publication is to allow
readers to gain a better understanding of the principles of distillation. After reviewing this
publication the reader will be able to apply the knowledge they acquire here and apply it to
more complex scenarios.

THE PROCESS OF SIMPLE DISTILLATION



Simple distillation is the most basic of all distillation techniques and is a fairly simple
process to understand. However, it is extremely important to understand the basics of
distillation and develop the necessary skills and knowledge before attempting any of the
other more complex techniques.

APPARATUS SETUP

Proper assembly of a distillation apparatus is essential in order to ensure a successful
distillation. For simple distillations users will use the following equipment:
Distillation flask (still): a closed vessel in which the solution to be distilled
is heated.
Three-way adapter: A connector with three ports that connects the
distillation flask to the condenser, and also allows users to insert a
thermometer into the system.
Condenser: A two chambered tube that cools product vapors using a water
jacket. It is very important to have the water inlet line attached to the
bottom port in order to evenly cool the vapor.
Vacuum adaptor: A curved tube connecting the condenser to the receiving
flask, which contains a port to attach a vacuum if needed.
Receiving flask: A closed chamber that collects the cooled distillate, often
accompanied by a ice bath to prevent re-vaporization of highly volatile
distillate
It is also very important when constructing the distillation apparatus to ensure that all
connections are tightly sealed. The use of a silicon-based grease will help to ensure that all
connections are airtight. The loss of vapor from leaks will result in low yields and can cause
contamination of the distillate. Below is a diagram depicting the correct setup of the
distillation assembly.

Figure 1: Proper distillation assembly for simple distillations 1


1 James W. Zubrick, The Organic Chem Lab Survival Manual, 4th ED. (1997)

PROCEDURE

Before adding the solution to the still it is extremely important to determine which
component of the solution is more volatile and note all components boiling points to
determine which component will vaporize first. After the boiling points have been
determined the solution can be added to the distillation flask and heat can be applied. As
heat is added, the user should closely monitor the vapors temperature and adjust the heat
source to prevent drastic heat spikes. Once the solution begins to bubble the temperature
should be held constant to prevent contamination of the distillate. It should also be noted
that the solution will begin to boil at an equilibrium point somewhere between the lower
and higher boiling points. This is due to the different vapor pressures of each component
and solutions vapor pressure/boiling point can be determined using Raoults Law:
=

As the solution continues to boil vapor will begin to move up the three-way adaptor and
move along the condenser. The condensation of the vapor is caused by the drastic change in
temperature caused by the cooling fluid. Depending on the component boiling points air can
be used as the condensing fluid, however it is more common to use water due to its higher
specific heat capacity, density, and conductivity. This allows water to transmit heat over
greater distances while using a much lower volumetric flow rate and temperature
difference compared to air-cooling. After the fluid completely condenses a liquid will begin
to drip/flow into the receiving flask.

As the distillate is collected the user should notice stabilization of the temperature reading.
During this temperature stabilization the most volatile component is boiling off and the
distillate collected is that component. After all of that component is collected there should
be a spike in temperature, at this point the collection flask should be removed to prevent
contamination, and a new one should be connected if the user is distilling a multicomponent
solution. Once all desired components are collected the heat source can be removed and the
apparatus can be disassembled once it has cooled.

SUMMARY

To summarize the simple distillation process, the process begins when a multicomponent
solution is charged into a distillation flask and is heated. Once the solution begins to boil
and the temperature stabilizes. The vapor will flow down the condenser, where it will be
cooled and be collected in a receiving flask. The distillate is collected until the temperature
begins to rise, at this point distillation is stopped or a new collection flask is added to collect
the next component. This process is repeated until all desired components are collected.