Amateur Aromatherapy

Distillation of Essential Oils

I know you don't want to here this but steam distillation of essential oils is
not really the territory of 'amateur' aromatherapists. Although I get a lot of
people asking me how to do it, I have never heard from anybody who has
successfully extracted more than a pin-sized drop of essential oil at home.
Perhaps they did not stay alive long enough after the boiler exploded to e-
mail me with the details. You can forget holistic therapy as you will need
some basic science, chemistry and some practical knowledge of the
fractional distillation process. Despite this, I'm sure you would be
interested in reading about it. As I don't work in the industry I have
cobbled this page together from references across the Web with some
smart-arse comments from me. So don't ask me technical questions as I
will not be able to answer them! I have included some appropriate
acknowledgements at the end.

"Distillation represents a dynamic part of a whole process where the

ethereal oils contained within a plants aromatic sacs or glands are
liberated through heat and pressure and transformed into a liquid essence
of sublime beauty. In a plants journey from seed to maturity, a constant
natural process of distillation is occurring as it draws into itself elements
from the surrounding environment and converts them into the substances
that give it life, structure, texture, color and fragrance. Harvesting the
plant at the appropriate time and endeavoring to distill from it the miracle
of its essence, is the high art and craft of the distiller."
Sounds good but how do we do it ?
"When considering the beauty and mystery of the world of aromatic plants
and their precious essences which are distilled and extracted by various
methods, one comes to realize that in the short space of a lifetime one
may only scratch the surface in understanding the subject. As all of you
know the process of growing any crop requires a lot of skill and knowledge
on the part of those engaged in such work. Working with nature over a
period of many years ingrains in one a respect for the wonders around one
and develops a sincere humility as learns to adjust to the environmental
changes that influence the growth of a plant from seed to maturity. When
plants have reached the moment of perfect aromatic maturity, they then
go into the hands of those engaged in distilling or extracting their precious
essence. It is one more vital part in the entire process. It is a subject that
has its own aura of mystery. Actually little has been written about the
intricacies of the subject and certainly one must be directly engaged in
this process to really understand it. The creative imagination will have to
serve for those of us who have not yet been afforded this opportunity."
Oh get on with it.
"First of all each and every aromatic raw material has to be considered as
an individual entity. The perfect time for harvest of some plants is more
straightforward than others. Flowers such as Rosa damascena, Jasminum
sambac, Jasminum grandiflorum, Citrus aurantium var.amara (Neroli),
must be plucked just as their buds are beginning to unfurl and at a very
specific time of day in order to capture the pure essences and produce oils
or absolutes of the highest quality. Once a flower has passed its prime
(which in most cases happens within a day or two) the essential oil quality
degrades quickly. Even in this case, there are some interesting facts to
consider. Some flowers have a bloom season of a month or less (Rosa
damascena) others can be as long as 6 months (Jasmin sambac) Whether
the season be long or short, there are some days within that period where
the the flowers have a balance of constituents which are considered the
most refined and perfect of all. But there are many plants where this is not
so. Consider the grasses like Lemongrass, Palmarosa Citronella, and
Gingergrass. The balance of their constituents changes from day to day as
they pass from mature grass to seed. Many times a specific balance is
required by large consumers of the oil and so test distillations are done
from day to day with immediate gc analysis being done to see what that
balance is. This is particularly true when particular components are being
isolated for for the flavor and fragrance industry. But one should not think
there is only one profile for a particular oil. There are often many different
profiles depending on not only the stage of maturity of the plant, but the
soil it is being grown in, the method of distillation, the length of time
between harvest and distillation, etc."
Sounds complicated. Maybe I'll just buy the oil rather than grow it myself.
"In examining this subject we also have to consider that in many
countries, a particular crop is not being grown by just one person on a
specific piece of land. Often there are large numbers of farmers growing
the crop on small land holdings. There may be a variety of cultural
practices employed by each that will influence the health and vigor of the
plants. Certainly the aromatic raw material will fit into certain parameters,
but it is important to realize that plants are greatly influenced by the
environment in which they live and even small differences in micro
climate, water, soil etc have their effect. Very few farmers have their own
distilleries and often the material growing in a certain local is taken to a
central facility where the material is distilled.
Prior to distillation the distiller may also be presented with the problem of
how to properly disintegrate or reduce in size (called comminution) the
material especially if he is dealing with dried aromatics like spices, seeds,
roots, etc. These materials have to be reduced in size so that during the
distillation process the maximum surface area of the plant material comes
in contact with the distilling/extracting medium (generally water, steam,
solvents, CO2) and release the volatile oils contained in the plants oil
glands or sacks. It is important that this be done in such a way that the
comminution process itself does not destroy the volatile oils (due to
excessive heat in grinding, crushing or slicing) or that their is not to much
lag time between the time when the plants are thus prepared and then
distilled (as when the aromatic materials are crushed,etc much
evaporation of natural oil can occur in a brief time). The ideal therefore is
to effectively and carefully reduce the size of the aromatic plant materials
so that the steam, boiling water can vaporize the maximum amount of
essential oil."
Sounds tricky as well.
"The cell walls of some plants are very thin and permeable which allows
steam, boiling water, solvents, etc to easily penetrate them, and carry
away the essential oil contained in the oil sacks or glands. But others have
to be carefully prepared before their essential oils can be released. Seeds
need to be thoroughly crushed and roots, stalks and woody material need
to be chopped into fine pieces. A whole range of comminution equipment
has developed to insure that this process is done in the most efficient and
sensitive manner. Some companies have even evolved crushing
equipment that disintegrates the material at sub freezing temperatures.
The main thing is that as soon as the crushing or grinding has occurred,
the distillation process should begin as the volatile oils rapidly evaporate
into the surrounding atmosphere.
Storage of plant materials prior to distillation is of importance to the
distiller. Many plant materials (dried roots, seeds, woods) can be
effectively kept for several months without significant loss of essential oil
content provided the room is cool, dark, dry and free from air circulation. If
these conditions are not meant then precious oil content can be lost due
to oxidation and resinification. Some plants like peppermint and clary sage
are sometimes partially dried before distillation as their very high water
content makes it difficult to distill in the fresh state. It was once thought
that there was little or no essential loss because of drying. But in fact this
has been proved wrong. There is a loss of essential oil in general and
specific components in particular. A detailed analysis of oil distilled from
fresh peppermint and partially dried peppermint will reveal a host of
differences especially in the minor and trace components. It does not
mean that the oil from partially dried material is not beautiful, it just
means that it is different."
Can an oil be beautiful ?
"Then of course there are the issues surrounding the type of equipment to
be used. Glass, aluminum, iron, stainless steel, and copper are all
common materials used in constructing stills of different sizes and shapes.
The still body itself (that is the vessel into which the raw material is
placed) can be designed to hold water, to have steam pumped into it,
have perforated plates upon which the materials sit, have automatic or
manually operated stirrers to prevent materials from sinking to the bottom
of the still and thus getting charred, etc.

Regarding distillation issues, some people say that glass is best, others
copper, others stainless steel, etc. It is an interesting debate because
those who follow a particular system have often attained high expertise in
what they are doing and the type of knowledge they have acquired and
the feeling for their equipment also greatly influences the quality of the
end product. It is true that the majority of oils are distilled with a more
commercial angle of vision. Large stills are created with efficient
condensers, etc and many mechanical controls are put in place to be sure
that the oils fit with the parameters of the international fragrance and
flavor industry (which produces the majority of the oils that are sold
today). But there are a growing number of small distillers who take great
pride in their art and craft and are constantly refining their techniques of
distillation so that the oils possess the greatest spectrum of aromatic
molecules as possible. In saying this I do not mean to say that the large
distilleries are devoid of such expertise. What they have accomplished in
terms of providing beautiful oils is no small achievement, but there is also
much to be said for the artisan working with their unit of 25-200 liters
distilling oils of superior quality. I think we shall see more and more of
these intimate endeavors arise in years to come."
Let's hope so but I don't want to pay a lot of money for a tiny bottle.
"Then when one gets into the world of the distillation itself, one has to
possess a tremendous amount of knowledge about the specific plants with
which one is dealing. One, either through intuitive knowledge or scientific
training has to understand the incredibly complex aromatic configuration
of the plant they are dealing with. Each plant possesses a range of
aromatic molecules from low boiling to high boiling constituents. The art
and craft of producing a truly amazing oil lies in understanding how to
"tweak" ones distilling techniques so that the the process captures both
the sublime top notes and the deep base notes. One has to know how to
bring up the heat in such a way that the material begins to release its
ethereal oil thus capturing the widest spectrum of molecules. This is
where the high art and craft of distilling takes on its most sublime form
and a person engaged in such aromatic creation happily devotes and
entire lifetime to perfecting their technique. For each and every raw
material that enters their still, they are having to discover the best
method for distillation. Indeed, one might say that few are the noses that
appreciate the nuances that they capture in their liquid gems. Most of us
are acquainted with very fine oils that are produced in commercial stills
but occasionally one comes across an artisan working on a more intimate
level and their oils may have a particular charging and beauty that cannot
be explained by any sophisticated mechanical analysis."
More craft than science ?
"In making an effort to appreciate the distillers art and craft one comes
cross a number of terms that require some effort to understand. Methods
of distillation include steam, water (sometimes called hydrodistillation),
water-steam, and hydrodiffusion. Extraction techniques include solvent
and CO2.
There are many technical terms which pertain to the operation of
distillation-vapour pressure, thermodynamics, boiling point, atmospheric
pressure, latent heat, hydrolysis, resinification, saturated steam,
superheated steam etc. Each term has a world of research behind it and
deserves careful study. It is beyond the scope of this modest introduction
to the subject to go into all the exact details. All that can be presented
here is a broad overview which is meant to instill in the heart a recognition
of some of the intricacies of the subject (and hence the wonder and
beauty inherent in it)"
Let's get started then.
"What does need to be understood about distillation though is that
whether one is doing water, water-steam, or pure steam distillation one is
going to be applying heat and pressure upon the aromatic tissues of the
plant and by the very nature of this exercise certain effects are produced
that are going to change the chemical nature of the essential oil as it
exists in the plant. The processes of diffusion, hydrolysis and thermal
decomposition do act upon the aromatic material during distillation
producing an oil which has some similarities and some differences from
the original. An essential oil should not be understood as something
perfectly representing the oil as it exists in the plant. It is what it is, a new
beautiful aromatic essence which arises as a result of many factors:
environment, individual plant characteristics, care and nurturing of the
farmer (watering, weeding, fertilizing, time of harvesting), proper
comminution of the material prior to distillation, distillation technique, the
understanding and awareness of the distiller, etc. In its highest form it is
like a great work of art which captures something of the exquisite beauty
of the living aromatic plant but is not the plant itself. It is an act of
creation arising from a long set of natural processes into which the human
element enters through taking a gift of nature and transmuting into a
sublime treasure which can be transported in a small vial to any place.
When the vial is opened releasing the trapped precious volatile vapors,
the effect it has is as powerful as the creative imagination of the person
inhaling it and the many processes that produced it.
From a simple outer standpoint-one can gain a comparative analysis of
the different systems of distillation (water, water and steam, and steam
distillation) by studying Book 1 of Ernest Guenther's 6 volume set called,
Essential Oils. In presenting his finding one has to take into account as
mentioned before, people that have developed an intimate knowledge of
their distillation technique may have risen above such observations as
Guenther makes."
Great. So now I need to buy a book.
These abbreviations will be used...
 WD = Water Distillation
 W/SD = Water and Steam Distillation
 SD = Steam Distillation

Types of Still

WD - Simple, low priced, portable stills; easily installed in producing

regions
W/SD - Somewhat more complicated and higher priced than WD. The
smaller type is also movable and may be installed in the field
SD - If well constructed, usually more solid and durable than than WD and
W/SD. Possibility of large size for large scale distillation
Types of Plant Material

WD - Most advantageous for certain materials, especially when finely

powdered; also for flowers which easily lump with direct steam. Not well
adapted for materials containing saponifiable, water soluble or high
boiling constituents.
W/S -Well Suited for herb and leaf material
SD - Suited for any charge except finely powdered material through which
the steam forms channels ("rat holes"). Especially well suited for seed,
root, and wood materials containing high boiling oils.

Modes of Comminution

WD - Best results with finely powdered materials

W/SD - Plant material must be uniformly but not too finely comminuted.
Granulation gives best results with seeds and roots
SD - Same as above

Modes of Charging

WD - Material must completely covered by water

W/SD - Material must be evenly charged into the still
SD - Similar to above. Proper charging is very important; otherwise the
steam channels through the plant materials and low yield results

Diffusion Conditions
WD - Good, if material is properly charged and moves freely in the boiling
water
W/SD - Good
SD - Good if steam is slightly wet. Distillation with superheated steam or
high pressure stem dries out the plant material, prevents diffusion, and
causes a low yield of oil. Such distillation must, therefore, be followed by
wet steam.

Steam Pressure Within the Still

WD - Usually about atmospheric

W/SD - Usually about atmospheric
SD - Can be modified (high or low pressure steam) according to the plant
materials

Temperature within the Still

WD - About 100 degrees Celsius. Care must be exercised not to "burn" the
plant material by contact with overheated still walls. Vaporized water be
continuously replaced
W/SD - About 100 degrees
SD - Can be modified (saturated or superheated steam) according to the
material.

Dry Steam - Steam that does not contain any unevaporated

water. "Dry, Saturated Steam", is dry and also at the boiling
temperature.

Wet Steam - Steam that contains unevaporated water as a

mist in the steam vapor.

Saturated Steam - Steam which is at the same temperature

as the boiling point of water at that pressure.

Superheated Steam - Steam which is at a temperature

above the temperature of boiling water at that pressure.
Therefore, Superheated Steam is always Dry Steam

Hydrolysis of Oil Constituents

WD - Conditions usually unfavorable. High rate of ester hydrolysis.

W/SD - Hydrolysis fairly low, provided no excessive wetting of the plant
charge within the still takes place.
SD - Conditions good, hydrolysis usually slight.

Guenther - "Hydrolysis in our case can be defined as a

chemical reaction between water and certain constituents of
essential oils. These natural products consist partly, and in
some instances largely of esters, which are compounds of
 organic acids and alcohols. In the presence of water,
particularly at elevated temperatures, the esters tend to react
with the water to from the parent acids and alcohols."

Conditions within the Plant Charge

WD - Good if plant material is covered with water and moves freely in it

W/S - Good if material is properly comminuted and charged. Prolonged
distillation causes excessive wetting by steam condensation and lumping
of the charges. Stills should be well insulated
SD - Conditions good, if plant material is properly charged,. Prolonged
distillation with wet steam causes excessive steam condensation with the
still and lumping of the charge

Rate of Distillation

WD - Relatively low
W/SD - Fairly good
SD - High

Yield of Oil

WD - In most cases relatively low, due to hydrolysis, also because water

soluble and high boiling oil constituents are retained by residual water in
the still
W/SD - Good, if no excessive wetting and lumping of the plant charge
occurs. This would prevent steam from penetrating the charge thoroughly
and result in abnormally low oil yield
SD - Good if plant material is properly comminuted, evenly charged, and
distillation properly conducted. Lumping of the charge or steam
channeling might cause abnormally low yield of oil

Quality of Oil

WD - Depends upon careful operation; "burning' of plant charge must be

avoided, especially when distilling with direct fire
W/SD - Usually good
SD - Good if operation properly conducted all around

Distillation Water

WD - Distillation water in some cases must be redistilled, or more

conveniently returned into the still during distillation (cohobation).
Distillation waters contain products of hydrolysis, chiefly
W/SD - If properly separated the distillation water can be discarded in
many cases
SD - Similar to above
Steam Boiler
The steam boiler is in most cases an oil or gas fired package boiler.
Biomass fired boilers are used in the Texas cedarwood oil industry, but
also quite common in remote third world areas. There however, some
distilleries purchase wood as a cheap local fuel, or burn fuel oil, while the
spent biomass of the process is discarded, primarily for being too wet.

Stills
Stills come in all sizes, shapes and materials of construction. A still is
basically a tank with some means of injecting steam at the bottom of the
tank in a way that allows its uniform distribution, such as perforated
crosses or plates, false bottoms, manifolds etc. This method is known as
"hydrodiffusion", as opposed to "hydrodistillation". In the latter, the still is
filled with the material submersed in water, and the oil is "boiled" out of
the aromatic raw material. A comparison of both processes was recently
described in a P & P article by M.H. Bolens. The opening of the still can be
a simple manhole cover or a full size lid with the same diameter as the
tank, depending on the unloading method. The steam/oil vapors exit at
the upper aids of the still or through an opening in the lid, which is
sometimes fitted with a coarse filter. Most stills operate at atmospheric
pressure, some are designed to stand higher pressures, in the 2 bar range.
The most popular unloading method is the basket-type (vetivert, Haiti),
some of which have several cross-sectional trays (flowers, France). Stills
that operate under pressure are sometimes unloaded under pressure
through a large opening at the end of a cone-shaped bottom (cedarwood,
Texas). Materials that require frequent loading and unloading are
processed in stills mounted on pivots which allow to swivel the still into
the upside down position and dump the entire content (lemongrass,
Guatemala). Some stills are mounted on dump trucks and taken to the
field for loading and unloading (mints, U.S.). Some stills are loaded and
processed directly in the fields by hydrodistillation (wild herbs, Morocco).

Condensers

Condensers are of various types. From truck radiators to copper coils; shall
and tube heat exchangers; pipes submersed in river fed canals; air cooled
condensers; tube condensers inside sprinkler towers, etc., depending on
the location, climate, available space and resources.

Oil Separators
The oil separator is the one component which is the most critical to the
overall product recovery and profitability of the plant, whether
conventional or continuous. Except in modern facilities, the separator
often seems to get the least engineering attention from distillery
operators in the field. The separator too, comes in a wide range of
homemade designs, although the main idea is that of a continuous
decanter sometimes referred to as a Florentine flask. Its efficiency is
governed by a number of well known variables; oil and water specific
gravity differential at various temperatures; phase viscosities versus
ascending and descending cross-sectional velocity at various distillate
flow rates and tank diameters; coalescing effects of different packing
materials; emulsification effects; oil solubility at various temperatures;
chemical composition and polarity of the oil and its effect on solubility,
etc. Distillers of heavy oils, such as vetivert, are usually much more aware
of the efficiency requirements of the separator than the distillers of light
oils such as citrus oils need to be.

Example of How To Operate a Home Still

Remember that at all times you will be dealing with the hot metal of the
retort and bird's beak. BE CAREFUL! It is advisable to wear gloves and eye
protection when operating your distiller.
1. Make certain valves for sight glass are in the open position. Turn counter clockwise.
2. Make certain the clean out valve is closed. (Perpendicular )
3. Plug for water inlet should be in place, at least hand tight.
4. It is recommended that the plugs for the heating element and the plug for the
submersible pump both be plugged into a serge protector. This will provide an on-off
switch. Never turn the heating element on unless there is water in the retort.
5. With the lid off and the inside basket in place, add plant material. Pack it as tightly as
possible. Once plant is inside the retort, add water. Add enough water to ensure that
the water level as evident in the sight glass is at least half way up the glass. Add the
water slowly .
6. After plant matter and water are in the retort, place the lid on top. Do not tighten the
lid as yet. The lid bolts should be in place but not tightened down.
7. Position the condenser. The legs of the condenser should be even with the legs on the
retort. The thermometer should be facing front. The spout on the condenser should be
facing front as well. Connect the condenser and the retort by tightening the Bird Beak
connector
8. Add water to the condenser. Water is either pumped in or piped into the bottom
nipple of the condenser. Water will exit from the nipple on top.
9. Turn on the heating element in the retort. It will take about 1/2 hour to build up
temperature. When water starts to boil, check the lid for steam leaks. if you discover a
steam leak, gently turn the lid bolt closest to the steam leak. Stop tightening when the
 leak ceases. There is no need to over tighten the lid. It is complete with a specially
designed gasket.

Distillation will take about 1 hour. The distillate should be captured in the
separatory funnel. In most cases, the essential oil will separate passively
and float to the top. The waters which have been separated can be
reintroduced into the retort through the water inlet at the top of the retort.
Steam will initially come out of the water inlet, but once you start pouring
water in the steam will exit elsewhere. BE CAREFUL!! This is very hot! Be
sure to wear gloves.
To clean your distiller allow the distiller to cool. Make sure the unit is
switched off, or unplugged. Disconnect the condenser first. Loosen the lid
bolts and remove the Bird’s Beak. Open the clean out valve. Hot water will
pour out the bottom. Remove the metal rods protecting the sight glass.
Lift the retort being careful to avoid breaking the glass. Tip the retort over
to empty the spent plant matter. Gently pull the handle of the basket to
remove plant matter. You can also leave the retort in place, and with the
bird's beak off, remove the plant material. Your spent plant material is
very hot. Wear gloves and BE CAREFUL!
If you plan to distill a different type of plant, you will need to clean the
still. This is easily done by adding water to the retort, connecting the
condenser (without circulating water) and turning on the heating element.
The water inside will boil, and the steam will clean out the retort and the
condenser. Steam will exit the condenser instead of distillate. Remember
to not add water to the condenser for cleaning purposes.

References
Most of the material taken from a White Lotus Aromatics newsletter.
http://members.aol.com/somanath/fragrant.html
Drawings of kit from The Food and Agriculture Organization of the United
Nations. http://www.fao.org/
Home stills from The Essential Oil Company.
http://essentialoil.com/distiller.html