The production of essential oils by steam distillation

Author: Ben Geurts

Date: April, 2019
Table of content

1 Introduction 3
2 Essential oils 4
2.1 Essential oils the formal definition 4
2.2 Chemical composition 4
2.3 The quality of essential oils 6
2.3.1 Growing and harvesting of plants (Rosemary) 6
2.3.2 Production 8
2.3.3 Storage and transport 9
3 Steam distillation 10
3.1 Water distillation 10
3.2 Wet steam distillation 12
3.3 Dry steam distillation 13
3.3.1 The steam boiler 14
3.3.2 The extraction column 16
3.3.3 The condenser 17
3.3.4 Oil water separator 18
3.4 Processing of end product 19

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1 Introduction

The start of the production of vegetable oils from fruits and grains goes back many years in the history of mankind.
Products like olive oil, sun flower oil and the like are known for centuries and are obtained by cold pressing of fruits
and seeds.
A nice example of this technique is the production of Argan oil. Today Moroccan women are still producing this
valuable product in a very traditional way by grinding the kernels of the fruits of the Argan tree (Argania spinosa) .

Pressing of oil from Argan nuts

The kernels are obtained by removing the flesh of the fruits. By first drying the fruit this goes more easily. Sometimes
the farmers allow goats to eat the fruit first and collect the kernels later from the droppings. Argan oil is a delicacy
in the Moroccan kitchen but is also used for the production of cosmetics.

Distillation is another very old technique that is used to make essential oils. There is evidence that already 1000 years
B.C. perfumes were made by distillation in Mesopotamia. In the old Arab world the production of rose oil and rose
water from the petals of the Damascus rose flower was already known.
Today we see a growing demand for natural products like lavender oil, rosemary oil, cedar oil, patchouli oil etc. The
cosmetic and pharmaceutical industry and their clients are more and more interested in pure and healthy products
obtained from whatever mother nature gives to us.
This document, that is provided by PUM Netherlands Senior Experts gives more background information about
producing essential oils from plants by steam distillation. Also subjects like the process economics and safety issues
of this process route will be addressed.

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2 Essential oils

What are essential oils?

Essential oils are fluids obtained from agricultural products that contain the very essence of a flower, a plant or a
tree in a very concentrated form. Many plants have a typical odour that gives us a pleasant experience. Without
seeing or touching we can recognise roses, lavender, rosemary, vanilla, coriander, cedar and many more plants just
by their odour.
It is obvious that in every garden we cannot plant a Eucalyptus tree. If you live in an apartment it is even impossible.
Yet, everybody loves the smell of Eucalyptus, in particular when you caught a cold. In short we like to surround
ourselves with pleasant fragrances.
In particular females appreciate the smell of flowers and all kind of herbs. In fact it were women that first started
to collect plants, flowers and herbs from the fields and forests to bring their fragrances into our homes Once we
learned to appreciate fragrances the need came to take pleasant odours with us. That was the time when the quest
for finding the very essence of fragrances began. Steam distillation was one of the techniques that were discovered
to concentrate fragrances in a portable form.

2.1 Essential oils the formal definition

According to the International Standard Organization on Essential Oils (ISO 9235: 2013) and the European
Pharmacopoeia (Council of Europe 2004) an essential oil is defined as the product obtained from plant raw
material by hydro distillation, steam distillation or dry distillation or by a suitable mechanical process (E.g.
for Citrus fruits)

The definition of an essential oil, given above, excludes other aromatic/volatile products obtained by different
extractive techniques like extraction with solvents (concretes, absolutes), supercritical fluid extraction, and
microwave-assisted extraction. Essential oils also differ from fixed oils or fatty oils in both chemical and physical
properties. Fatty oils contain glycerides of fatty acids and leave a permanent stain on filter paper, whereas essential
oils contain volatile compounds and vanish rapidly without leaving any stain. Essential oils are complex mixtures of
volatile and semi-volatile compounds, usually with a strong odour, rarely coloured and soluble in organic solvent
however insoluble in water.

2.2 Chemical composition

Modern chemistry enables us to identify the main components of essential oils. Besides these main components
essential oils may contain a lot of other components that are typical for certain species which may have an influence
on their odour. Below the main components of some well-known oils are listed:

Lavender
Lavender oil is an essential oil obtained by distillation from the flower spikes of certain species of lavender.
Two main forms are distinguished, lavender flower oil from e.g. the Lavandula augustifolia, a colourless oil, insoluble
in water, having a density of 885 g/l; and lavender spike oil, a distillate from the herb Lavandula latifolia, having a
density of 905 g/l.

Lavandula augustifolia Lavandula latifolia

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The main components of Lavender oil of these two species are;

Component Lavandula augustifolia Lavandula latifolia

Linalool 28.92 % ww% 49.47 ww%
Linalyl acetate 32.98 ww% -
Eucalyptole 25.91 ww%
Camphor 0.85 ww% 13.00 ww%

It is interesting to observe the physical properties of the main components in their pure form:

Component Melting point Boiling point Liquid density Solubility in water

°C °C g/l g/l
Linalool < -20.0 198.0 858.0 1.6
Linalyl acetate < 0.0 220.0 895.0 0.03
Eucalyptole 2.9 176.0 922.5 3.5
Camphor 179.0 204.0 990.0 1.2

It is observed that:

• The main components are all poorly soluble in water. This make it easy to separate the oil from water after
condensation
• The densities of these components are all lower if compared to the density of water. This indicates that
Lavender oil will stay on top of the water phase after condensation.
• The boiling points are all high. This tells us that with steam distillation the vapour phase is mainly water
containing only a small fraction of oil vapours.

Rosemary
Rosemary oil is extracted from the fresh flowering tops of the Rosmarinus officinalis, commonly known as Rosemary.
It is a woody, perennial herb with fragrant, evergreen, needle-like leaves and white, pink, purple, or blue flowers,
native to the Mediterranean region.

Rosmarinus officinalis

The main components of Rosemary oil are:

Component Rosmarinus officinalis

-Pinene 9.04 % ww%
Eucalyptole 35.86 ww%
Camphor 15.75 ww%
-Terpineol 6.42 ww%

It is to be noted that some of the main components of Lavender oil and Rosemary oil are the same:

Component Melting point Boiling point Liquid density Solubility in water

°C °C g/l g/l
-Pinene -62.8 156.9 858.0 0.16
Eucalyptole 2.9 176.0 922.5 3.5
Camphor 179.0 204.0 990.0 1.2
-Terpineol -35.9 215.0 913.0 2.42

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Also here we see that:

• The main components are all poorly soluble in water. This make it easy to separate the oil from water after
condensation
• The densities of these components are all lower if compared to the density of water. This indicates that
Rosemary oil will stay on top of the water phase after condensation.
• The boiling points are all high. This tells us that with steam distillation the vapour phase is mainly water
containing only a small fraction of oil vapour.

Eucalyptus
Eucalyptus oil is extracted from the leaves of the Eucalyptus tree. The tree, Eucalyptus tereticornis, is original from
Australia but several varieties of this tree can be found all over the world. The scent of this tree is well known an d
repels mosquitos.

Eucalyptus tereticornis

The main components of Eucalyptus oil are:

Component Eucalyptus (Average 7 species)

-Pinene 7.50 % ww%
Eucalyptole 73.09 ww%

It is no surprise that the main component of Eucalyptus oil is Eucalyptol also called 1,8 Cineole which gives the oil
its typical fresh smell.

2.3 The quality of essential oils

The quality of essential oils is an important aspect to be considered. Because essential oils are a product from mother
nature the quality is influenced by the way the raw materials (plants) are treated, the way in which they are processed
(The distillation process) and the way in which they are stored. The clients, to which the product is transported, have
different quality criteria. It makes a big difference if essential oils are being used for making cosmetics or
pharmaceutical products. Each product has its own specific characteristics that needs to be tested for its application.
In general quality control starts with keeping track of what happens during the whole production cycle starting with
the harvest of plants in the field end ending with storing the end product in bottles.
As an example some guidelines are given below for the quality control of the production of rosemary oil.
We will use rosemary as an example in this syllabus because rosemary can be found in many countries.
2.3.1 Growing and harvesting of plants (Rosemary)

The best quality Rosemary oil is obtained from the fresh picked flowers. Rosemary oil when distilled from the
flowering tops has a clear, powerful refreshing minty-herbal smell with a woody, balsamic undertone. This oil is
colourless or slightly yellow with a water like viscosity. Many producers cut and distil the entire plant, however this
oil will have a higher camphor content and is definitely inferior in quality to the above. The practice to distil the
flowering tops separately is more labour intensive but will obtain essential oil with a better market price.
Usually, farmers will deliver plants by truck in sewn plastic bags. Each delivery from a farmer is called a batch and
should be labelled and stored in a separate place not to be mixed with materials from other farmers.

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A convenient way to store and transport the delicate material is to put it in big bags. Below a picture of a standard
type big bag is given with a volume of 1000 l (1m3)

The big bag keeps the material inside clean and free from dirt. This is very convenient for storage. Big bags may be
stacked. Products of different suppliers can be kept aside in the distillation plant. Big Bags can be reused several
times and are available in many types, qualities and sizes.
For the storage and transport of plant material a bag with a big opening on top and a discharge spout at the bottom
is very convenient. Once the bag is filled it can be closed with a knot. In the distillation plant it can be transported
and emptied easily using a fork lift truck or a hoist.

On the bag a label can be attached on which the following information can be given:

• Latin name of the plant species: e.g. Rosmarinus officinalis

• Place of harvest
• Date of harvest
• Batch number or bar code

With the batch number or bar code a unique number should be given which may be traced bag to the origin of the
content of the bag.

Below an example is given:

Batch number is : Specie code + Year + Harvest date + Farmer code + Bag number
XXXX 2019 0306 YYYY 0067

With this unique number the farmer may give more detailed information, so called meta data, which can be send by
email to the production plant.

One may think of the following information:

• Day of shipment
• Key to translate specie code to Latin name
• Key to translate farmer code to place of harvest
• Information with respect to the use of crop protection agents
• Net weight of the bag
• Content : Leaves + stem or flower tops only

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In general the use of crop protection agents should be avoided if possible. In particular if the essential oil is used for
pharmaceutical applications. In case the use of crop protection agents cannot be avoided care should be taken in
selecting a safe agent.

2.3.2 Production

The best quality rosemary oil is obtained from the flowers. The flowers have a strong odour that attracts bees. The
bees bring the pollen from the stamens to the pistil that is hidden deep inside the flower. The bees are rewarded for
their work with nectar. The odour comes from the essential oil therefore it is obvious that the flowers have the
highest essential oil concentration.

The leaves also contain essential oil but the concentration is lower. The stem, in particular, if it looks like wood,
contains hardly essential oil and contains components that have a less favourable odour.

Good starting material for the distillation process are fresh dried flowers and leaves. If possible drying should take
place at a moderate temperature and preferably not too long in the hot sun. At a high temperature the flowers and
leaves may already loose some essential oil.

During the distillation process we have to make sure that the temperature will not rise to much and that we use “dry”
steam. This will be discussed in more detail in the next chapter.

At the end of the distillation process the essential oil may contain some moisture. Make sure to remove this by drying
the oil with a drying agent. See also next chapter.

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2.3.3 Storage and transport

Rosemary oil is a delicate product that may lose its quality if not handled and stored properly. Heat, light and air are
direct enemies that will attack the oil.
Make sure that the oil is stored in bottles that protect the content against direct sun light. Below an example of a
good storage bottle is shown.

The bottle is made from dark brown glass and the cap closes the bottle air tight. Finally the bottles should be stored
in a cool place. In case the product needs to be stored for a longer period before dispatch it should be stored in an
air conditioned warehouse.

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3 Steam distillation

In the previous chapter we have seen that the main components of essential oils are chemicals with a high boiling
point. A high boiling point does not mean that we can heat up our raw materials (e.g. flowers or leaves) to a very
high temperature. Most organic compounds are sensitive to heat and will decompose at high temperatures. Therefore
we use steam. Hot steam causes the cell walls of the plant material to break up to release the essential oils. The
evaporated essential oil is evaporated by the steam and is then cooled down in a condenser. A mixture of water and
liquid oil is now dripping from the condenser and collected in a separating vessel. Because the oil is (usually) lighter
than water, a water layer and oil layer will be visible. The separation vessel is designed in such a way that the oil
layer and water layer can easily be separated. The oil that is obtained in this way is called crude essential oil.
Depending on the quality of the crude oil, additional finishing operations may take place such as filtration or drying.

Why using steam for distillation?

There are several reasons to use steam for the production of essential oils:

• Steam is a medium that can also be used for cleaning and sterilizing our equipment. This is in particular useful
for the pharmaceutical application of the oil.
• Steam has a high heat of evaporation (± 2100 kJ/kg) that will facilitate the evaporation of the essential oil
which has a much lower heat of evaporation.(e.g. the heat of evaporation of Eucalyptol is only 260 kJ/kg).
• Water is an environmental friendly raw material
• As mentioned earlier most essential oils are not soluble in water which makes it easy to separate the product
from the water.

There are different types of steam distillations that will be discussed in more detail below:

1. Traditional water distillation

2. Steam and water distillation
3. “Dry” steam distillation

3.1 Water distillation

Water distillation is the traditional way of making essential oil. There is evidence that the Arab physician and
philosopher Ibn Sina, also known as Avicenna, was using this technique as early as 1000 A.D.

Below a very old picture is shown of a simple water

distillation also called Alembic. Further down a picture
is shown of a copper distillation unit. The whole
apparatus was usually made from copper. The copper
kettle on the left was filled with water and the petals
of flowers (E.g. Rose petals). On top of the kettle a
condenser pipe is mounted. The pipe is bended
downwards to a glass bulb in which the condensate,
water + oil, is collected.
A fire is lit underneath the kettle and the water starts
boiling. Once the water is boiling two processes take
place at the same time. The first process is the
dissolving of water soluble material. Water solvable
components are salts and certain organic compounds.
The second process is the evaporation of components
that are not soluble in water like the essential oils. The
essential oils are picked-up by the steam and leave the
kettle at the top via the condenser pipe. In the old days the condenser was a copper pipe that simply was cooled
down by air. The condensate is collected in a glass bottle. The condensate is a mixture of oil and water. The oil stays
on top and can be collected by decantation.

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Copper Alembic

In this way 3 products are obtained:

1. The concentrated water remaining in the kettle

2. The essential oil (Top product)
3. The condensed water (Bottom product)

Normally the concentrated product in the bottom of the kettle has no value. The rose oil is the product with the
highest value. The condensed water is called hydrosol water.

The advantages of water distillation are:

• Simple process like boiling tea

• Process works at atmospheric pressure
• Kettle can be heated in several ways
• Often used for small scale production.

Disadvantages of water distillation:

• The process is slow and the distillation time is much longer there by consuming more firewood / fuel thus
making the process not economic.
• The heating rate of the furnace is difficult to control
• The yield is low if compared to other steam distillation techniques.
• The plant material at the bottom of the kettle is in direct contact with the hot bottom which makes it very
likely that it will char giving a bad odour to the product
• A long heating time may cause the hydrolysis of esters to form organic acids and alcohols
• The production method is less suitable for large and commercial scale production
• Water distillation is not suitable for high boiling hard roots an wood like plant material

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3.2 Wet steam distillation

This type of distillation is already a big improvement of the water distillation. The plant material is no longer boiled
in the kettle but is placed in a compartment above the kettle.

Improved steam distiller

The bottom of this compartment has a support grid of fine woven metal that prevents the material of falling down
into the kettle. When the kettle is fired the steam rises up through the bed of plant material and evaporates the
essential oil. The oil and water condense in the condenser and can be separated easily. The steam that is produced
in the kettle is saturated steam This type of distillation is already a big improvement if compared to water
distillation. There are field units on the market with processing capacities ranging from 100 – 2000 kg of pant
material per batch.

The advantages of the wet steam distillation are:

• A higher yield
• A better quality oil
• Less fuel consumption because of a shorter distillation time
• No charring of material on the bottom of the steam kettle

The disadvantages of the wet steam distillation are:

• More expensive equipment

• Water droplets entrained in the wet steam may come in contact with the plant material this decreases the
quality of the end product
• When fired with wood or dried left over material it remains difficult to control the distillation

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3.3 Dry steam distillation

Dry steam distillation is the industrial solution for optimum control of the steam distillation process.
In this system the whole distillation unit is split into 4 different sections:

1. The steam boiler which produces superheated dry steam.

2. The extraction column in which the plant material is placed.
3. The condenser
4. The oil water separator

The water distiller and wet steam distiller are both operated at atmospheric pressure. Hence the steam temperature
will never be higher than the boiling point of water and is always wet. With a steam boiler we are able to make steam
with a higher pressure and a higher temperature. Below a graph is shown with the saturated steam temperature as a
function of the steam pressure.

Saturated steam temperature versus steam pressure

160

150
Steam temperature [°C]

140

130

120

110

100
1 1.5 2 2.5 3 3.5 4 4.5 5 5.5 6
Steam pressure [bar]

E.g. at a pressure of 3.6 bar we can make steam with a temperature of 140 °C. After expansion of the steam to a
lower pressure the steam will no longer be saturated but superheated. We call this “Dry” steam.

Example

In a steam boiler saturated steam is made with a pressure of 3 bar. In the graph above we can read that the steam
temperature is 133.5°C. We send this steam to the extraction column which has a pressure of 1 bar (Atmospheric
pressure). Because of the expansion of the steam the temperature of the steam will drop to 122 °C. This is 22 °C
above the saturated steam temperature at atmospheric pressure which is 100 °C. (Boiling point of water)

Working with “Dry” steam means that we have created a tool to control the temperature in the extraction column.

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3.3.1 The steam boiler

The operation of a steam boiler asks for special attention because the unit is operated under pressure. For all
equipment that is operated under pressure special regulations are applicable. In most countries there a regulations
with respect to the design and manufacturing of steam boilers. In Europe this is outlined in the Pressure Equipment
Directive (PED). In addition to this steam boilers need at regular intervals inspections by certified organisations to
make sure that they can be operated safely.
Steam boilers are available for several heat sources such as gas, oil, wood, coal and/or agricultural waste material.
For small size boilers even electric power is an option in particular if electric power can be obtained for free via Solar
panels. For countries with a lot of sun shine every day, this is certainly an option that could be very interesting. For
small size steam boilers with a capacity below
1000 kg/h the operating pressure is normally 8 bar abs. with a saturated steam temperature of 170 °C.
Some important aspects of using and selecting a steam boiler are explained below:

Selection of the required boiler capacity

The capacity of the steam boiler that is needed depends on the diameter of the distillation tower. Normally the steam
load of the extraction tower is between 120 – 240 kg/h.m2 . Below a table is given:

Boiler capacity [kg/h] Energy inpuy [kW]

Tower diameter [mm]
min max min max
100 0.9 1.9 0.9 1.7
200 3.8 7.5 3.5 7.0
300 8.5 17.0 7.9 15.7
400 15.1 30.2 14.0 27.9
500 23.6 47.1 21.8 43.7
600 33.9 67.9 31.4 62.9
700 46.2 92.4 42.8 85.6
800 60.3 120.6 55.9 111.8
900 76.3 152.7 70.7 141.5
1000 94.2 188.5 87.3 174.6

Control of the steam flow

A good control of the steam flow to the extraction column makes it possible to obtain first class distillation results.
The capacity control depends on the type of fuel that is used. Below an illustration is given of a modern steam
boiler:

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In the furnace gas, oil, wood, coal or bio mass is burned. The hot flue gas from the furnace flows through tubes.
The tubes are immersed in the water of the boiler and transfer the heat of the flue gas to the water that will start
boiling. If we need more steam we give more fuel to the furnace. If we need less steam we give less fuel to the
furnace. When using gas or oil as a fuel control is quick and almost immediate.
However a furnace that is operated with solid fuel material like wood, coal or biomass does not react so quickly.
We need to control the heat with letting in more or less air into the furnace. Also adding the fuel is a manual
operation an need to be watched carefully. Therefore these type of furnaces are only used when the fuel material
is cheap e.g. the material that is left over after the distillation.

The water balance of the boiler

The water that is evaporated in the boiler and transferred to the extraction column causes the water level in the
boiler to drop. In a modern steam boiler water is supplied at the bottom of the boiler and the water level is
controlled automatically. As soon as the water level drops a valve in the water supply line is opened to take in fresh
water. Once the level is restored again this valve closes again. In case of manual control there should be a sight
glass from which the operator can observe the water level in the boiler.

Safety

In the past many accidents happened with steam boilers. Special regulations for pressure equipment see to it that
steam boilers are well designed and equipped with safety devices. The main safety problems with steam boilers
arise in the following situations:

1. A very high pressure

2. Boiler running dry

A boiler is made of steel and is designed to withstand a certain maximum pressure. Above this pressure the kettle is
ruptured. When we continue to heat the boiler without using steam the pressure can rise above the design pressure
of the boiler. Therefore, by law, a safety valve must be mounted on every steam boiler (See picture below:

The bottom nozzle of the valve is mounted on top of the boiler. A spring keeps a certain pressure on the disc that
keeps the valve closed. The pressure at which the valve opens can be regulated by adjusting the screw on top of
the valve. In case the pressure is rising above the safety value the disc will lift and the steam will flow directly to
the open air. The arrows indicate the direction of the steam flow.
A safety valve is a valve that is carefully designed for every steam boiler and comes with a certificate. This
certificate clearly states the relief capacity of the valve and a test protocol. Although there is a screw on top of the
valve this may never be adjusted by the user of the boiler. To make sure that nobody will do this the screw is
marked with red lacquer. Only authorised personnel may adjust this screw.

A boiler that is running dry may lead to serious damage or even rupture of the pipe bundle. To avoid this boilers
should be safeguarded with a low water level switch. First an alarm is given that the water level is dropping
quickly. If no action is taken the switch will automatically stop the fuel supply to the furnace.

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It is to be noted that a furnace with solid fuels cannot be stopped immediately. Therefore special safety measures
must be taken to avoid overheating of the boiler.

Water quality

Water quality is important for the operation of a steam boiler. Normal tap water is not suitable for use in a steam
boiler. Tap water always contains some salt (even if we don't taste it) and in some parts of the world it can contain
a lot of lime. Because the water in the boiler evaporates, the salt concentration of the water that remains in the
boiler will increase. If the concentration becomes too high, this will lead to corrosion of the boiler pipes, and lime
will also deposit on the pipe bundle. This is also the case if the boiler is made from stainless steel. In particular a
high chloride concentration may lead to severe corrosion problems. Lime deposit will decrease the heat transfer of
the hot flue gas to the water in the boiler. Eventually this may even lead to pipe rupture. To decrease the salt
concentration a part of the water in the boiler must be purged at regular intervals. Special boiler feed water
treatment units are available to make tap water suitable for use in a boiler. Also anti corrosion agents are available
on the market that can be added to the boiler feed water. It is recommended to seek advice from companies
specialised in boiler feed water treatment.

3.3.2 The extraction column

The extraction of the essential oil takes place in a column that is filled with a bed of plant material. At the bottom
of the column a support grid covered with a steel mesh prevents the material from falling down and enables the
steam to flow through the bed. Below a picture of an extraction column is shown:

The plant material is dropped via an opening at the top into the column. There is as steam connection at the
bottom and at the side of the column. The connection at the side is used for keeping the wall of the column warm
to prevent steam from condensing at the wall.
At the end of the extraction process the column is emptied by opening the bottom. The help of a hydraulic cylinder
makes this easy. There are other types of extraction columns in which the plant material is put into a basket. The
basket has also a support grid and a steel mesh at the bottom. The basket is lowered into the column via the top. At
the end of the extraction process the basket has to be hoisted out of the column via the top. With 2 extraction
columns placed side by side it is possible to switch the steam supply from one column to the other. While one column
is in operation the other column can be emptied and refilled. During the filling of the column, it is necessary to
ensure that the plant material is uniformly distributed

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Column control

The distillation column is controlled with the steam flow and the steam pressure. The choice of the optimum steam
flow depends on the product that is handled. In the next chapter we will go into more details with respect to the
distillation of rosemary. In general the following rule of thumb can be used:

• A too low flow will start condensation of steam in the column. This gives a poor product quality and will
increase the overall distillation time that is needed.
• A too high flow gives the steam not enough time to come in contact with the plant material. It does not
speed up the distillation process and we use too much energy which makes our product expensive.

During the distillation process the first oil is produced in the bottom of the column as soon as this layer is exhausted
the production moves on further to the top of the column. Therefore we start the process with a low steam
pressure (Low superheated steam) at the end of the distillation we increase the steam pressure (High superheated
steam) to make sure that we also evaporate the essential oil in the top of the column.
3.3.3 The condenser

The traditional condenser is a pipe that as winded as a spiral and submerged under water.

The steam and oil vapours from the distillation column flow through the tubes. The condenser is filled with water
and a continuous supply of fresh water sees to it that the steam and oil are condensed.

In today’s industry the standard type condenser is a shell and tube heat exchanger.(See below)

Cooling water inlet

Vapour inlet

Condensate outlet Cooling water outlet

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In school we learned that energy (heat) cannot be destroyed. So let us assume that the whole distillation is
a black box in which we put energy at a high temperature (Steam is the energy we put into the system). The energy
(heat) we put into this box has to come out. It will come out in the condenser because heat always flow from a
place with a high temperature to a place with a low temperature The cold cooling water we supply will pick up the
heat that is coming from the distillation column. By doing so the cooling water itself will heat up. Off course we do
not want the temperature of the cooling water to go up to much. Therefore we maintain a steady flow to keep the
temperature rise between 5 – 10 °C. Below a table is given that indicates the cooling water that is needed to
condensate the steam that is needed for distillation columns of several sizes:

Boiler capacity [kg/h] Energy inpuy [kW] Cooling water capacity [l/h]
Tower diameter [mm]
min max min max min max
100 0.9 1.9 0.9 1.7 75 151
200 3.8 7.5 3.5 7.0 302 604
300 8.5 17.0 7.9 15.7 679 1358
400 15.1 30.2 14.0 27.9 1207 2415
500 23.6 47.1 21.8 43.7 1886 3773
600 33.9 67.9 31.4 62.9 2716 5433
700 46.2 92.4 42.8 85.6 3697 7395
800 60.3 120.6 55.9 111.8 4829 9658
900 76.3 152.7 70.7 141.5 6112 12224
1000 94.2 188.5 87.3 174.6 7546 15091

Note: Cooling water temperature rises from 20 °C to 30 °C

Small distillation units may use tap water as cooling water for bigger units a cooling water tower is needed.
When using tap water or water from a cooling water tower care should be taken when the water contains a lot of
lime. After some time lime will deposit on the outside of the tubes and this will reduce the cooling capacity of the
condenser. Also dirt in the cooling water will reduce the cooling capacity.
Lime scaling may be removed from the tubes by cleaning the shell side of the condenser with a mild acid. There are
suitable products on the market for descaling equipment.

Control of the condenser

Condenser control is easy. At the beginning, after starting the supply of the cooling water, we watch carefully the
outlet temperature of condenser. Once we are sure that the condensed steam and oil has a temperature below
45 °C we keep the cooling water flow constant and may turn or attention to the control of the other operating
conditions.
3.3.4 Oil water separator

One of the earliest methods of separating the essential oil and the water was invented in Florence (Italy). It is called
the Florentine flask. A picture of a historical Florence flask is shown below:

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Date: April, 2019
There are 2 types of separators. One for oil lighter than water and one for oil heavier than water. The principle of
separation is easy. Oil and water are not mixable. Therefore the liquid with the highest density remains at the
bottom of the separator and the liquid with the lowest density on top. In a glass bottle or a bottle with a sight glass
one can clearly see the separation between the 2 layers.
For most distillation processes the oil remains on top. The water flows via the like a swan neck shaped pipe out of
the bottle and may be collected in a separate vessel. As soon as a sufficient thick oil layer is formed this may be
drained to a crude oil collection vessel via the outlet at the top of the separator.

The same principle as the Florentine flask is still used on a bigger scale. In the picture below this is shown:

Water + Oil

Water Oil Oil

For a good separation of oil and water time is needed. In the industrial size separator two Florentine flasks are
connected in series to make sure that oil is completely separated from the water.

3.4 Processing of end product

At the end of the process the “crude” essential oil is collected in a vessel. The processing of the end product begins
with the inspection of the crude oil. There are of course extensive laboratory tests that we can do to check the
quality of the crude oil. But there are also simpler tests that already give a good indication of the quality of our
product. Below are a few given focused on rosemary oil:

1. Rosemary oil has no colour or has a faint yellow colour.

2. When put on a white sheet of paper it should show no stains after drying.
3. The measure density is in the range between 0.894 - 0.912 g/ml at 25 ºC
4. The refractive index is in the rage between: 1.464 - 1.476 at 20 ºC
5. The product is completely soluble in alcohol

The density and refractive index can be measured with simple equipment. (See pictures below)

Refractive index meter Pycnometer

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Date: April, 2019
But before putting the oil into bottles 2 more steps are needed:

• Removal of suspended solids

• Removal of water

The oil may contain some suspended solids such as remains of the plant material or rust particles. Suspended solids
can be removed by filtration. Water can be removed by adding a suitable salt that can absorb the water (E.g. water
free gypsum) Once the water is absorbed, the salt it be removed via filtration.

Finally the clear and dry essential oil may be bottled, labelled and stored in a cool area.

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Date: April, 2019