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Murray Hunter – University Malaysia Perlis                                ESSENTIAL OILS




                            The distillation of
                             essential oils 2:                                                                                     PART


     Part two of this three part series on distillation carries on from the basic principles laid out in part one to look
           at the stages of the general distillation process and outlines the various basic types of distillation.

Distillation occurs in a number of definable                              Stage one                                    Stage two                              Stage three
stages. During the first stage, initial heating
occurs through the charge where the plant
material has been placed. Plant material                                                     Linalool
will not be saturated with moisture and the
temperature differential between the steam
                                                     Percentage increase of the distillate




and the plant material will allow quick
                                                                                                                              Methyl chavicol
dissipation of latent heat from the steam to
the plant material. The initial steam,
particularly if it is wet will tend to cool
throughout the lower layers of the charge,
where some condensation may occur. This
has to be watched carefully, as too much
                                                                                                         1,8 Cineole
condensation may flood the lower parts of
the charge. Dry superheated steam may
have the effect of drying out the plant
material. Both flooding and drying out of
the plant material are detrimental to
efficient distillation. At this early stage
steam is the only contributor to vapour                                                      Eugenol
pressure until saturation occurs and the
layering process, discussed above begins.
    The second stage begins when the                                                                    Progressive number of constituents
vapour reaches the condenser. At this point
the oil-to-water ratio will be at its highest.     Figure 1: The distinct stages of distillation, and during the second phase, for sweet basil oil.
During the second phase the distillation
process will go through three sub-phases.          the change in composition of sweet basil                               the vat and the plant material surfaces
ɀ In the early stage, due to some effect           oil during distillation.2                                              area within the charge. The rate of steam
    from relative volatilities of the various          The height of the still will influence this                        flow per hour is subject to the amount of
    constituents, the most volatile                phenomenon. High stills tend to negate                                 plant material in each charge. Daily
    constituents will tend to vaporise first       this effect because as the more volatile                               throughput is thus limited by the amount of
    and carry a higher than proportionate          constituents from the bottom layer reach                               steam that can be generated on an hourly
    weight in the distillate as compared to        the top layer, the less volatile constituents                          basis at a distillation plant. Steam must
    the normal oil. It is also reported that       from the bottom layer will have already                                also be adjusted to suit the absorptive
    oxygenated constituents also have a            started distilling over and reaching the                               capacity of the plant material. This greatly
    tendency to distil over before                 upper layers of the charge.                                            varies between different herbs and the
    hydrocarbons.1                                     The final stage of distillation occurs                             condition they are in before distillation.
ɀ During the middle stages, the oil will be        when the water-to-oil ratio is very high as                               Steam produced by high pressure
    distil over in the same proportions as         the charge becomes exhausted of oil. It will                           external boilers is usually very dry and can
    the normal oil, and                            no longer be economical to continue with                               often be superheated. Steam produced by
ɀ During the third stage, the least volatile       the distillation.                                                      medium pressure boilers around 3
    constituents of the oil will contribute a                                                                             atmospheres pressure will contain
    higher than proportionate composition in       Steam and pressure                                                     moderate moisture content, but will not
    the distillate.                                For efficient distillation, i.e., achieving the                        tend to superheat. Steam produced from
                                                   maximum amount of oil with the minimum                                 evaporators at atmospheric pressure is
The distinct stages of the second stage            quantity of steam, requires the maximum                                relatively moist. In water-steam distillation
distillation can be seen in Figure 1 showing       exposure between the steam flowing into                                array where steam is produced in the same

                                                                                                                          July 2012 P E R S O N A L C A R E           67
ESSENTIAL OILS


vessel that the plant material is stored will     that the temperature gradient increases,              Recently a variation on the operation of
produce very wet steam.                           thus increasing the effects of latent heat         pressure in steam distillation has been
    Different steams can be utilised as a         exchange and reduces the likelihood of             reported a number of times, utilising a
control mechanism to correct the                  hydrolysis. However the use of high                technique called instantaneous controlled
conditions within the still housing the plant     pressure distillation is limited by the extent     pressure drop (DIC). This is a technique
charge.                                           that prolonged high temperatures will              where the foliage is first exposed to
    Wet steam is a saturated vapour is            damage the composition of the essential            saturated steam and then the pressure
suitable for most distillation. In most cases,    oil.                                               drastically dropped to a vacuum level of
wet steam from a water bath produces ‘a                Inversely, as operating pressure is           around 5-50 KPa to provoke auto-
richer oil’ with much shorter extraction time     reduced, so does the temperature of the            vaporisation of the superheated volatile
than other forms of steam.3 This is               distillation. This method can be used for          compounds through expanding and
particularly the case with plant material         the extraction of heat sensitive constituents      breaking up the cell walls with
that contains superficial oil glands.             that would normally be damaged through             instantaneous cooling.4 Experiments have
Increasing steam rates does not speed up          exposure to excess heat. However                   shown that results can be varied through
distillation, especially if the process of        distillation under reduced pressure has a          changing time, pressures and the amount
hydro-diffusion is required. As plant             number of limitations. Steam under                 of moisture in the leaves.5
material is already saturated with moisture       reduced pressure is less dense, so requires
and there is a constant diffusion rate. If        more steam to carry out a distillation than        Wilting crops before
herbs contain a lot of moisture, then there       under normal atmospheric pressure. The             distillation
would be sufficient moisture in the plant         condenser system would need to be                  As the moisture condition of the herb is a
material to commence hydro-diffusion and          almost twice the size of a conventional still      factor in the efficient distillation of the
dry steam would be the most suitable to           or a refrigeration system required in              herb, wilting is often carried out to dry the
apply. However dry steam has less mass            condensing the distillate. The recovery            crop before processing. The objective of
than wet steam and as such reduces the            vessel and separator would have to be              wilting is to dry the herb enough to
latent heat of steam, thus prolonging the         sealed within the closed system, which             increase its absorptive surface. Many
distillation period.                              would lead to design and engineering               practitioners believe it is to dry out excess
    A superheated steam occurs when the           difficulties.                                      moisture so that distillation will be shorter
temperature of the vapour is higher than
that of the same saturated vapour at the
same pressure. Superheated steam is
independent of pressure and therefore
advantageous in a number of situations, as
it can be utilised at any temperature
without increasing pressure, i.e., can
increase the temperature of distillation
without having to change the steam flow-
rate due to changes in pressure.
Superheated steam can be used for drying
out a flooded charge vessel, where there is
too much liquid around the plant material.
However superheated steam is not
advisable for general distillation as it would
dry out the plant material, preventing the
hydro-diffusion process occurring and is a
poor conductor of latent heat – two of the
important processes needed for efficient
distillation. Superheated steam is most
suitable for the distillation of glabrous herb
material and can increase yields
substantially.
    High boiling oils exert less vapour
pressures and require relatively large
temperature gradients to extract them
during distillation. This leads to prolonged
distillation periods. If the constituents are
stable under long periods of heat,
distillation can be performed under
pressures above the atmosphere, which
increases temperature. This cuts back on
distillation time and saves energy. As
increasing the still pressure, increases
temperature, the temperature gradient will
also increase between the vapour space in
the still and the plant material. This assists
in the vaporisation of high boiling volatile      Figure 2: Mint foliage, cut and laid on the ground for wilting, being picked up by the harvester
constituents. The advantage of pressure is        for distillation at Myrtlefor, Victoria.

68            P E R S O N A L C A R E July 2012
ESSENTIAL OILS


and more efficient. However this is a
                                                                                                      Condenser cooling
fallacy. For example, with tough leaves like
                                                                                                         water outlet
eucalyptus and tea tree, wilting does little
to dry them out or increase their surface                                                                                 Vapour condenser
absorption, so wilting will have no benefit
to the distillation process. Moisture in the
                                                                                 Vapour outlet
plant material is actually of benefit to the                                     to condenser
distillation process.6 In fact there are risks
with wilting in that the process may lead to                                                                        Condenser cooling
                                                                               Still chamber for                       water inlet
losses in oil, not through evaporation, but
                                                                                plant material
through chemical reactions like oxidisation,                                       (loaded by
resinisation and the formation of glycosides                                        cartridge,
and enzymes in the materials. Excessive                                           or directly)
drying of moisture can remove necessary
moisture breaking the contact between the                                         Welded wire
                                                                                                                                            Separator
oil component and surface of the plant               Steam inlet                  mesh floor
                                                                                                                                              flask
material, thus hindering the promotion of            from boiler                     Steam outlet
hydro-diffusion during the distillation
process.
    Which crops require wilting before                                          Still drain valve
distillation generally depends upon their
natural surface absorption capacity. Non-        Figure 3: Diagram of a steam distillation still.
absorptive herbs like mint and basil need
some wilting to promote absorption during        which need to be comminuted before                   become part of the boiling mixture and
distillation, as wilting to promote partial      distillation, like almond powder and huon            resulting mixed vapour.
breakdown of the surface cellular structure      pine saw dust.                                           As water boils and converts to steam at
of the leaf. In this case distillation would        In water distillation there are a number          the bottom of the vat and rises through the
then commence with a wet steam fraction,         of simultaneous processes that act to                plant charge, it will come into contact with
followed by slightly drier steam once            extract volatile constituents from plant             the plant material. Some oil is exposed on
moisture has permeated into the leaf             material that are different from steam               the surface of this material will be
structure. Herbs with absorptive surfaces        distillation.                                        vaporised by the rising steam as it comes
like lavender do not need to be wilted. In          Essential oils contain a number of                into contact with the plant surfaces. This
fact they do not have enough moisture to         oxygenated constituents that are relatively          steam carrying some volatile vapour will
link the oil glands to the surface via a water   soluble in water. This would include                 rise to the surface and carry over into the
interface, so wet steam fractions are            phenols, alcohols and some aldehydes.                vapour space above the water until it
needed during distillation. Grass crops like     During the early stages of a water                   reaches the still condenser.
lemongrass and citronella contain enough         distillation, these compounds would                      The boiling temperature of water at the
moisture within their leaf structure to          dissolve in the surrounding water and                bottom of the vat in water distillation is
create a water-oil-surface interface for
hydro-diffusion to occur during distillation,     Table 1: Some common water soluble aroma chemicals in essential oil.
so wilting is not necessary. As moisture
content is already sufficient in the leaf, dry    Slightly soluble                    Moderately soluble              Very soluble
steam would be suitable for the distillation      (<500 ppm)                          (501-1999 ppm)                  (>2000 ppm)
process.                                          Aldehyde C11                        Calamene                        Benzlaldehyde
                                                  Aldehyde C12 (lauric)               1,8-Cineole                     Benzyl acetate
Water distillation
                                                  Aldehyde C12 MNA                    Nerol                           Cinnamic alcohol
Water distillation involves distilling plant
material totally immersed in water.               Amyl cinnamic aldehyde              Neryl acetate                   Citronellyl acetate
Depending upon the specific gravity and           Amyl salicylate                     Rose oxide                      α-Copanene
charge mass in the still, the material will       Benzyl salicylate                                                   Eugenol
either float or sit totally immersed in the       Cedrol                                                              Geranial
water. Heat is introduced by direct heating       Citronellol                                                         Geraniol
of the sides of the vat, a steam jacket, a
                                                  Citronellyl butyrate                                                Limonene
closed system coil or in some cases a
perforated steam coil. Water distillation was     Citronellyl formate                                                 Linalool
the only method used before the 20th              Eudesmol                                                            Mentone
century.                                          Geranyl formate                                                     Myrcene
    Water distillation is useful for the          Limonene                                                            (E)-β-ocimene
distillation of flower materials which would      Linalyl acetate                                                     Phenylethylacetate
normally congeal and form lumpy masses
                                                  α-Pinene                                                            Phenylethylalcohol
under steam distillation, where steam
would not penetrate, like rose petals and                                                                             Sabinene
orange blossoms. This method is also                                                                                  Terpinen-4-ol
useful for fruit kernels that would form                                                                              α-Terpineol
glutinous masses under steam distillation                                                                             Terpinolene
and powdered forms of plant material

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ESSENTIAL OILS


slightly less than the boiling point of water,      the plant surface material as possible             material from directly coming into contact
due to the mixed liquid of solublised               during the distillation.                           with the heating coils.
volatiles and water. Heat applied to the still          The effects of hydro-diffusion are much            With many materials, part of the oil
will cause the creation of a small bubble of        slower in water than other types of                dissolves in the water during distillation and
saturated mixed vapour from the liquid              distillation. Consequently, especially for         forms a milky emulsion, as a number of
phase, where upon formation it rises to the         wood materials extensive comminution               aromatic constituents are soluble to some
top of the water in the charge. During the          must be undertaken so that particles in the        degree in water. This loss could range up to
rise, the bubble’s pressure, temperature            charge are fine and as much oil as possible        25% of the essential oil.7 This means that
and proportion of oil to water decreases.           is exposed on the surface of the material.         the recovery of oil is incomplete and the
The condensing volatiles, mostly being less             In water distillation, plant material is       recovered oil will be deficient in some
dense than water, float to the top of the           placed in a sealed vessel or retort that           constituents that would be the case with
water and form a film on the surface of the         connects directly to a condenser. From the         the oil recovered through steam distillation.
water in the vessel. This lost oil tends to         condenser the distillate runs into a               Upon separation in water distillation, the
remain on top of the surface and cannot             separator. The rate of distillation is             water distillate is returned directly to the
re-vaporise easily due to its higher boiling        controlled by the intensity of the fire, the       charge vessel to replace the decreasing
point and the generally cooler temperatures         pressure of the vessel or retort and/or the        water level due to evaporation. This is
at the water surface. Most of the oil               rate of introduction of steam. As many             called cohobation. Sometimes the water
recovered in water distillation is the portion      woods contain high boiling compounds,              distillate is redistilled in another vessel to
of the oil that does not condensate through         pressure is vital to create high enough            extract the volatiles in emulsion. Salt is
this action.                                        temperatures to vaporise the volatile              often added to the distillate to reduce the
    Observation shows that distillation             constituents. These constituents may take          solubility of water. Whether this process is
undertaken with vigorous boiling produces           many hours to boil out. Hydro-stills should        undertaken depends upon the probability of
better and quicker yields than mild boiling.        generally be wide to maximise the                  the constituents being damaged by further
Some distillers even install small propellers       evaporation area. Where particles are fine         heat and the economics of re-distillation.
intruding into the side of the still to assist      such as saw dust and powders some form             Another method to recover the dissolved
in agitation. This is most probably effective       of mesh or “P” shape pipe arrangement              aromatic materials from the water distillate
because the agitation in the charge tank            should exist at the entrance to the                is to add a solvent. The mixture is then
prevents oil droplets clinging to the herb          condenser to prevent plant material from           vigorously shaken to pick up dissolved
surfaces. It is necessary to generate               entry and possible clogging. Heavy charges         constituents from the water into the
enough steam in the water so that it will           and where heat coils are used in the still         solvent. These materials are then recovered
come in contact with as much of the oil on          require a perforated grid to prevent plant         through vacuum distillation of the solvent

 Table 2: A comparison between water, water and steam and steam distillation.

                                   Water distillation                  Water and steam distillation              Steam distillation
 Construction                      Usually simply constructed,         Inside vat contains a grill where         Utilises an outside steam source
                                   based on ancient designs.           plant material rests above the water
 Plant material suitability        Finely powdered materials such      Can be used for most herb and             Most materials, except fine
                                   as woods and rhizomes, flowers      leaf materials. Material must             powders. Good for high boiling
                                   that congeal with steam.            be packed in a uniform                    materials. Material must be packed
                                   Not suitable for materials that     manner to avoid channeling                in a uniform manner to
                                   contain acidic material which can   of steam.                                 avoid channeling of steam.
                                   saponify, water soluble or
                                    high boiling constituents.
                                   Material must be completely
                                   covered with water.
 Hydro-diffusion                   Excellent                           Good                                      Steam should be slightly wet to
                                                                                                                 promote diffusion. Superheated or
                                                                                                                 high pressure steam can dry out the
                                                                                                                 plant material and inhibit diffusion.
 Available Pressure                Atmospheric pressure                Atmospheric pressure                      Can be adjusted for both high and
                                                                                                                 reduced pressures.
 Available Temperature             100˚C, but care must be taken       Approximately 100˚C                       Can be increased or reduced
                                   not to burn the plant material                                                according to pressure used.
                                   from direct heat on the sides.
 Hydrolysis Condition              Usually a high rate of ester        Hydrolysis is usually low, however        Slight hydrolysis.
                                   hydrolysis.                         excessive wetting of the plant material
                                                                       through prolonged distillation can
                                                                       promote hydrolysis during later
                                                                       stages of distillation.
 Rate of distillation and yield    Slow rate of distillation.          Moderate distillation rate.               Fast rate of distillation.
                                   Low rates of yield due to           Good yields if no channels                Good yields if no channels
                                   hydrolysis and loss of water        occur in charge. Usually good yields.     occur in charge. Usually good yields.
                                   soluble constituents into the
                                   water. High boiling constituents
                                   often left undistilled.



70              P E R S O N A L C A R E July 2012
ESSENTIAL OILS


which results in a secondary essential oil.8
Some common water soluble aroma
chemicals in essential oils are listed in
Table 1.
    Another method that will contribute to
minimising oil loss due to oil solubility in
water during the separation phase is to
control the outgoing distillate temperature
from the condenser. Where oils are less
dense than water, there will be an optimal
temperature range where oil particles will
freely float to the top of the distillate upon
condensation. Some literature on
distillation practices misses the point about
the effect of condensation temperatures on
oil yields.9 Based on private work,10 the
higher the temperature of the outgoing
distillate, the freer will be the oil particles
to float to the top. For example, tea tree oil
droplets will float to the top of the water
distillate twice as fast at 60°C than at
40°C. The upper temperature limit will be
restricted by the potential loss of low
boiling volatiles during condensation. This
has implications on the design of the             Figure 4: The condenser, with the end manifold removed to expose the internal cooling pipes,
specific condenser for specific crops and         at the author’s property in Perlis, Malaysia.
set range limits upon the temperature that
distillation can take place, to achieve a         water distillation. Water and steam              steam distillation facilities are designed and
specific outgoing distillate temperature          distillation has another advantage over          built with the correct steam ratings, they
range.                                            steam distillation as there are fewer            are much more economical to run than
                                                  decomposed products during the process           water and water and steam distillation
Water and steam distillation                      due to less chance of plant material drying      systems. A comparison between water,
Water and steam distillation involves the         out. However water and steam distillation        water and steam and steam distillation is
storing of the plant material above a water       will take a lot longer. Water and steam          shown in Table 2. below.
bath situated in the bottom of the charge         distillation can produce very good results
vessel and heating the water either through       under reduced pressure.                          The condenser system
direct fire, a steam jacket or a closed or            Water and steam distillation is much         A condenser in an essential oil distillation
open steam coil. Water and steam                  cheaper to set up than steam distillation        system is a heat exchange or dissipating
distillation produces saturated wet steam at      facilities and lends itself to portable stills   device. The condenser must not only cool
the prevailing vessel pressure, which is          that can be transported from place to            the condensate vapour into a liquid, but
usually atmospheric pressure. Within this         place.                                           also cool the condensate to the
configuration, unlike water distillation, only                                                     temperature range where the oil will
steam comes in contact with the plant             Steam distillation                               separate spontaneously from the water.
material.                                         Steam distillation employs an external               The usual array for a condenser system
   Water and steam distillation is not very       steam generation system, external to the         is a tube or set of tubes running through a
suitable for fine materials as steam will find    charge vessel. This configuration provides       sealed water reservoir to cool the pipes. It
a path of least resistance tending to create      much more control (depending upon the            is immediately attached to the top of the
channels. This means that steam will not          boiler capacity) than water and steam            charge vessel to collect all vapour exiting
flow through the whole mass of plant              distillation. This is because in steam           the vessel. The design of the condenser
material and an incomplete distillation will      distillation the wetness fraction,               must ensure that the vapour flow is
take place. If the plant material is loosely      temperature and pressure can be                  turbulent inside the tubes to prevent high
packed, the same effect will happen, as           manipulated according to needs and               velocity vapour freely flowing through the
the material will offer no resistance to the      conditions. However, it is a misconception       condenser and maximise exposure to the
steam.                                            that greater steam volumes and increased         cooler walls. A baffle is usually installed at
   Water and steam distillation may take a        pressures have positive effects on the           the beginning of the condenser to disrupt a
long period of time to reach operating            process in all cases. As mentioned               straight steam flow for this purpose. Failure
temperature as the plant material needs to        previously, dry and superheated steam has        to achieve those conditions would result in
be heated up with only saturated steam.           the effect of drying out plant material,         some vapour failing to condensate. Within
This may cause early condensation and             which potentially halts distillation through     the condenser system the flows of vapour
wetting of the plant material.                    the stopping of hydro-diffusion process.         and cooling water should be in opposite
   Due to the limits on pressure that can         Faster steam flow rates do not necessary         directions at the maximum possible speed.
be built up in the charge vessel, water and       mean quicker recovery times. Fabricated          The condenser must be sensitive enough to
steam distillation will have only a limited       steam boilers cost much more to run than         react on the vapour flow very quickly. The
effect on extracting high boiling materials       water baths and may lead to high                 required number of tubes and length of the
from plant materials. However there is less       distillation costs, especially if they require   condenser depends on the rate of distillate
opportunity for hydrolysis to occur than with     petrochemical feed stocks. However if            flow, the pressure, the temperature of the

                                                                                                   July 2012 P E R S O N A L C A R E             71
ESSENTIAL OILS


cooling water and the desired exit                                                                   microscopic oil droplets. Temperature plays
                                                   Distillate in-flow from still
temperature range of the distillate.               (water-oil mixture)                               a crucial role in separation, where it should
   The condenser must remove the                                                                     be moderately warm to increase the
equivalent amount of heat that is needed                                                             relative specific gravity differential of the oil
to vaporise the distillate, plus the additional                       Oil                            and water. Raised temperature of the
                                                                     outlet
amount of heat to reach the optimal                                                                  distillate water will allow the small oil
distillate temperature range of the                                                                  particles to rise to the top of the separator
condensate distillate exiting the condenser.                                                         quicker in a similar manner to the
The rate of which heat would be removed                                                              condenser exit temperature range where
from the distillate can be represented by                                                 Water      there will be an optimal separator water
                                                                  Internal                outlet
the following equation:                                            baffle                            temperature range to promote oil-water
   Q = UA∆t  ∆                                                                                       separation.11
   Where Q = the heat removed by unit                                                                    During distillation, the more volatile
   of time                                                                                           constituents tend to vaporise quicker and
   U = a constant determined by                                                                      the less volatile constituents vaporise later
   operating conditions (condensing and                                                              in the distillation. This leads to an oil that
   cooling made up of a number of                                                                    will vary in constituents during the
   factors) usually a constant is used.                                                              distillation period. By changing separation
   A = the area available for heat                                                                   flasks at particular points during a single
   removal                                                                                           distillation, oils of different constituent
   ∆t = the temperature difference                                                                   profiles can be collected. This is important
   between the vapour and the cooling             Figure 5: Schematic view of a hydro-diffusion      in ylang ylang and lavender distillation,
   medium.                                        distillation system.                               where different oils profiles will have
                                                                                                     different uses and values to particular
U is made up of a number of factors               possible separate the oil from the distillate      customers. Many distillers also use this
including the flow rates of cooling water         water. As distillate water volume is much          principal to collect specific fractions during
and vapours, the material that the                greater than oil, it is important that water       the distillation, which can later be blended
condenser is constructed, and usually a           can be removed continuously. Oil and               together to create a whole oil that meets
constant is used due to the difficulty to         water separates according to specific              with certain specific specifications, such as
calculate. The value of U increases as            gravity forming two layers. Lighter than           a standard.
these factors increase. Thus according to         water oils will float to the top and heavier           The water distillate will always be
the equation, the surface area can be as          than water oils will sink to the bottom. This      saturated in oil and directly dumping it
large or small as desired, as long as the         must be considered in separator design for         would lead to a loss in yield. For this
other factors compensate. However the             water removal.                                     reason some distillers (water and water and
overall capacity of the distillation system          If the specific gravity of oil and water is     steam distillation) will channel the water
will have great bearing on the condenser          very close, the two components will not            distillate back into the still vessel for re-
area. Condenser sizes will also vary in size      separate immediately. Distillate flowing into      distillation in what is called cohobation,
according to the temperature of available         the separator must therefore not disturb           mentioned previously. For this purpose the
cooling water on site, thus condensers in         the surface area and flow into the body of         separator must be placed higher than the
temperate and tropical areas will reflect         the water to prevent surface turbulence.           still vessel proper so distillate water in the
this in size.                                     The separator must also be large enough            separator can be fed back into the still
    Using a condenser system with the             so that drained water does not carry away          through gravity.
wrong capacity for the distillation system
will have a number of operational
                                                                                          Steam inlet
consequences. A too efficient condenser
system will deliver the distillate at a
temperature below the optimum range,
which could lead to cool air outside being                                                                           Downward steam flow
sucked into the system. This outside cooler
air in the condenser tubes could create
expansion and contraction of vapours in                                                                              Plant material
the condenser leading to splattering and
                                                      Side opens so that
intermittent distillate outflow. This could           cartridge with plant
also occur if the cooling water is too cold.          material can slide in                                          Grated base
If the condenser is too small for the                   and out of still
distillation system, then the still must be
operated with lower steam rates, which
                                                                                                                     Condenser array
would lengthen distillation times and open
up the possibility of hydrolysis to occur
within the vessel.
                                                                                                                     Water and oil collector
The separator system
Before leaving the subject of distillation in
this chapter, some words about the                                                                                   Collector vessel
separator system must be mentioned. The
function of the separator is to as quickly as     Figure 6: Oil separator design used in Perlis, Malaysia.

72            P E R S O N A L C A R E July 2012
ESSENTIAL OILS


Hydro-diffusion                                    material near the bottom may also lead to              6 Guenther E.The Essential Oils, Volume One:
distillation                                       hydrolysis and lead to lesser yields.                     History – Origin in Plants, Introduction – Analysis,
Hydro-diffusion distillation is a variation on     However, hydro-diffusion distillation appears             Malabar, Florida, Robert E. Krieger Publishing
steam distillation where steam is                  popular within the aromatherapy industry in               Company, P 110, 1948.
                                                                                                                          .
introduced on the top of the vessel and            Europe.                                   PC           7 Fleisher A. Water-soluble fractions of the
condenses through the plant material in                                                                      essential oils, Perfumer & Flavorist 1991;
the still, where the distillate is collected       ɀ The final article in September will                     16 (3): 37-41.
and condensed under the plant material               conclude with a brief discussion about               8 Bouzid N, Toulgouate K, Villarem G, Gaset A.
which rests on a grill or perforated tray.           applying these principles.                              Analyse quantitative des fractions d’huile
Through steam travelling down the still,                                                                     essentielle pouvant co-exister lors
there is more time for the volatiles and           References                                                d’hydrodistillation de plants aromatiques,
fatty acids floating on the plant material.        1 Johannes AK, Scheffer JC, Svendsen AB.                  Rivista Ital Eppos 1997; 79: 15-25.
In the case of wood and seeds that have              Comparison of Isolation Procedures for Essential     9 Boland DJ, Brophy JJ, House APN. Eucalyptus
many high boiling compounds, which are               Oils, Z. Lebensm. Unters. Forsch, Vol. 168,             Leaf Oils: Use, Chemistry, Distillation and
difficult to vaporize in an ordinary still, this     1979, pp. 106-111.                                      Marketing 1991; Melbourne, Inkata Press, P    .
system may be effective. This would be             2 Private communication with Mr. Jon Bonnardeaux          191.
valuable when fatty acids contribute to the          of Western Australia Department of Agriculture,      10 Unpublished private work on tea tree distillation
flavour of a material and it is desirable in         early 1990s.                                            at Batu 9, Berseri, Perlis, Malaysia during
the oil. Thus, hydro-diffusion distillation        3 Denny EFK. Field Distillation for Herbaceous Oils,      2004/5.
may return an oil more representative of             Lilydale, Tasmania, Denny McKenzie &                 11 Hughes AD, (1952), Improvements in the Field
the plant’s natural profile.12                       Associates, P 81, 1990.
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    It is reported that hydro-diffusion            4 Kristiawan M, Sobolik V, Al-Haddad M, Allaf K.          Engineering Experimental Station Bulletin No. 31
distillation gives quicker distillations with        Effect of pressure drop on the isolation of             1952; Oregon State College, 1-64.
lower steam consumption than                         cananga oil using controlled pressure drop           12 Legast E, Peyron L. Hydrodiffusion Industrial
conventional steam distillation.13 However           process, Chemical Engineering and Processing            Technology to Produce Essential Oils by
this process is governed by the physical             2008; 47 (1): 66-75.                                    Steam, in Proceedings of the 11th International
laws that govern any other type of                 5 Rezzoug SA, Boutekedjiret C, Allaf K.                   Congress of Essential Oils, Fragrances
distillation and the fact that the steam             Optimization of operating conditions of rosemary        and Flavors Vol. 2 1989; New Dehli, India,
travels downwards while cooling may affect           essential oil extraction by a fast controlled           69-73.
the transfer of latent heat and thus                 pressure drop using response surface                 13 Hall R, Klemme D, Nienhaus J. The H&R Book:
increase, rather than decrease distillation          methodology, Journal of Food Engineering 2005;          Guide to Fragrance Ingredients Vol. 4 1985
time. The tendency to saturate the plant             71 (1): 9-17.                                           London, Johnson Publications, P 13. 0
                                                                                                                                               .




                                                                                                          July 2012 P E R S O N A L C A R E                  73

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The Distillation of Essential Oils Part 2

  • 1. Murray Hunter – University Malaysia Perlis ESSENTIAL OILS The distillation of essential oils 2: PART Part two of this three part series on distillation carries on from the basic principles laid out in part one to look at the stages of the general distillation process and outlines the various basic types of distillation. Distillation occurs in a number of definable Stage one Stage two Stage three stages. During the first stage, initial heating occurs through the charge where the plant material has been placed. Plant material Linalool will not be saturated with moisture and the temperature differential between the steam Percentage increase of the distillate and the plant material will allow quick Methyl chavicol dissipation of latent heat from the steam to the plant material. The initial steam, particularly if it is wet will tend to cool throughout the lower layers of the charge, where some condensation may occur. This has to be watched carefully, as too much 1,8 Cineole condensation may flood the lower parts of the charge. Dry superheated steam may have the effect of drying out the plant material. Both flooding and drying out of the plant material are detrimental to efficient distillation. At this early stage steam is the only contributor to vapour Eugenol pressure until saturation occurs and the layering process, discussed above begins. The second stage begins when the Progressive number of constituents vapour reaches the condenser. At this point the oil-to-water ratio will be at its highest. Figure 1: The distinct stages of distillation, and during the second phase, for sweet basil oil. During the second phase the distillation process will go through three sub-phases. the change in composition of sweet basil the vat and the plant material surfaces ɀ In the early stage, due to some effect oil during distillation.2 area within the charge. The rate of steam from relative volatilities of the various The height of the still will influence this flow per hour is subject to the amount of constituents, the most volatile phenomenon. High stills tend to negate plant material in each charge. Daily constituents will tend to vaporise first this effect because as the more volatile throughput is thus limited by the amount of and carry a higher than proportionate constituents from the bottom layer reach steam that can be generated on an hourly weight in the distillate as compared to the top layer, the less volatile constituents basis at a distillation plant. Steam must the normal oil. It is also reported that from the bottom layer will have already also be adjusted to suit the absorptive oxygenated constituents also have a started distilling over and reaching the capacity of the plant material. This greatly tendency to distil over before upper layers of the charge. varies between different herbs and the hydrocarbons.1 The final stage of distillation occurs condition they are in before distillation. ɀ During the middle stages, the oil will be when the water-to-oil ratio is very high as Steam produced by high pressure distil over in the same proportions as the charge becomes exhausted of oil. It will external boilers is usually very dry and can the normal oil, and no longer be economical to continue with often be superheated. Steam produced by ɀ During the third stage, the least volatile the distillation. medium pressure boilers around 3 constituents of the oil will contribute a atmospheres pressure will contain higher than proportionate composition in Steam and pressure moderate moisture content, but will not the distillate. For efficient distillation, i.e., achieving the tend to superheat. Steam produced from maximum amount of oil with the minimum evaporators at atmospheric pressure is The distinct stages of the second stage quantity of steam, requires the maximum relatively moist. In water-steam distillation distillation can be seen in Figure 1 showing exposure between the steam flowing into array where steam is produced in the same July 2012 P E R S O N A L C A R E 67
  • 2. ESSENTIAL OILS vessel that the plant material is stored will that the temperature gradient increases, Recently a variation on the operation of produce very wet steam. thus increasing the effects of latent heat pressure in steam distillation has been Different steams can be utilised as a exchange and reduces the likelihood of reported a number of times, utilising a control mechanism to correct the hydrolysis. However the use of high technique called instantaneous controlled conditions within the still housing the plant pressure distillation is limited by the extent pressure drop (DIC). This is a technique charge. that prolonged high temperatures will where the foliage is first exposed to Wet steam is a saturated vapour is damage the composition of the essential saturated steam and then the pressure suitable for most distillation. In most cases, oil. drastically dropped to a vacuum level of wet steam from a water bath produces ‘a Inversely, as operating pressure is around 5-50 KPa to provoke auto- richer oil’ with much shorter extraction time reduced, so does the temperature of the vaporisation of the superheated volatile than other forms of steam.3 This is distillation. This method can be used for compounds through expanding and particularly the case with plant material the extraction of heat sensitive constituents breaking up the cell walls with that contains superficial oil glands. that would normally be damaged through instantaneous cooling.4 Experiments have Increasing steam rates does not speed up exposure to excess heat. However shown that results can be varied through distillation, especially if the process of distillation under reduced pressure has a changing time, pressures and the amount hydro-diffusion is required. As plant number of limitations. Steam under of moisture in the leaves.5 material is already saturated with moisture reduced pressure is less dense, so requires and there is a constant diffusion rate. If more steam to carry out a distillation than Wilting crops before herbs contain a lot of moisture, then there under normal atmospheric pressure. The distillation would be sufficient moisture in the plant condenser system would need to be As the moisture condition of the herb is a material to commence hydro-diffusion and almost twice the size of a conventional still factor in the efficient distillation of the dry steam would be the most suitable to or a refrigeration system required in herb, wilting is often carried out to dry the apply. However dry steam has less mass condensing the distillate. The recovery crop before processing. The objective of than wet steam and as such reduces the vessel and separator would have to be wilting is to dry the herb enough to latent heat of steam, thus prolonging the sealed within the closed system, which increase its absorptive surface. Many distillation period. would lead to design and engineering practitioners believe it is to dry out excess A superheated steam occurs when the difficulties. moisture so that distillation will be shorter temperature of the vapour is higher than that of the same saturated vapour at the same pressure. Superheated steam is independent of pressure and therefore advantageous in a number of situations, as it can be utilised at any temperature without increasing pressure, i.e., can increase the temperature of distillation without having to change the steam flow- rate due to changes in pressure. Superheated steam can be used for drying out a flooded charge vessel, where there is too much liquid around the plant material. However superheated steam is not advisable for general distillation as it would dry out the plant material, preventing the hydro-diffusion process occurring and is a poor conductor of latent heat – two of the important processes needed for efficient distillation. Superheated steam is most suitable for the distillation of glabrous herb material and can increase yields substantially. High boiling oils exert less vapour pressures and require relatively large temperature gradients to extract them during distillation. This leads to prolonged distillation periods. If the constituents are stable under long periods of heat, distillation can be performed under pressures above the atmosphere, which increases temperature. This cuts back on distillation time and saves energy. As increasing the still pressure, increases temperature, the temperature gradient will also increase between the vapour space in the still and the plant material. This assists in the vaporisation of high boiling volatile Figure 2: Mint foliage, cut and laid on the ground for wilting, being picked up by the harvester constituents. The advantage of pressure is for distillation at Myrtlefor, Victoria. 68 P E R S O N A L C A R E July 2012
  • 3. ESSENTIAL OILS and more efficient. However this is a Condenser cooling fallacy. For example, with tough leaves like water outlet eucalyptus and tea tree, wilting does little to dry them out or increase their surface Vapour condenser absorption, so wilting will have no benefit to the distillation process. Moisture in the Vapour outlet plant material is actually of benefit to the to condenser distillation process.6 In fact there are risks with wilting in that the process may lead to Condenser cooling Still chamber for water inlet losses in oil, not through evaporation, but plant material through chemical reactions like oxidisation, (loaded by resinisation and the formation of glycosides cartridge, and enzymes in the materials. Excessive or directly) drying of moisture can remove necessary moisture breaking the contact between the Welded wire Separator oil component and surface of the plant Steam inlet mesh floor flask material, thus hindering the promotion of from boiler Steam outlet hydro-diffusion during the distillation process. Which crops require wilting before Still drain valve distillation generally depends upon their natural surface absorption capacity. Non- Figure 3: Diagram of a steam distillation still. absorptive herbs like mint and basil need some wilting to promote absorption during which need to be comminuted before become part of the boiling mixture and distillation, as wilting to promote partial distillation, like almond powder and huon resulting mixed vapour. breakdown of the surface cellular structure pine saw dust. As water boils and converts to steam at of the leaf. In this case distillation would In water distillation there are a number the bottom of the vat and rises through the then commence with a wet steam fraction, of simultaneous processes that act to plant charge, it will come into contact with followed by slightly drier steam once extract volatile constituents from plant the plant material. Some oil is exposed on moisture has permeated into the leaf material that are different from steam the surface of this material will be structure. Herbs with absorptive surfaces distillation. vaporised by the rising steam as it comes like lavender do not need to be wilted. In Essential oils contain a number of into contact with the plant surfaces. This fact they do not have enough moisture to oxygenated constituents that are relatively steam carrying some volatile vapour will link the oil glands to the surface via a water soluble in water. This would include rise to the surface and carry over into the interface, so wet steam fractions are phenols, alcohols and some aldehydes. vapour space above the water until it needed during distillation. Grass crops like During the early stages of a water reaches the still condenser. lemongrass and citronella contain enough distillation, these compounds would The boiling temperature of water at the moisture within their leaf structure to dissolve in the surrounding water and bottom of the vat in water distillation is create a water-oil-surface interface for hydro-diffusion to occur during distillation, Table 1: Some common water soluble aroma chemicals in essential oil. so wilting is not necessary. As moisture content is already sufficient in the leaf, dry Slightly soluble Moderately soluble Very soluble steam would be suitable for the distillation (<500 ppm) (501-1999 ppm) (>2000 ppm) process. Aldehyde C11 Calamene Benzlaldehyde Aldehyde C12 (lauric) 1,8-Cineole Benzyl acetate Water distillation Aldehyde C12 MNA Nerol Cinnamic alcohol Water distillation involves distilling plant material totally immersed in water. Amyl cinnamic aldehyde Neryl acetate Citronellyl acetate Depending upon the specific gravity and Amyl salicylate Rose oxide α-Copanene charge mass in the still, the material will Benzyl salicylate Eugenol either float or sit totally immersed in the Cedrol Geranial water. Heat is introduced by direct heating Citronellol Geraniol of the sides of the vat, a steam jacket, a Citronellyl butyrate Limonene closed system coil or in some cases a perforated steam coil. Water distillation was Citronellyl formate Linalool the only method used before the 20th Eudesmol Mentone century. Geranyl formate Myrcene Water distillation is useful for the Limonene (E)-β-ocimene distillation of flower materials which would Linalyl acetate Phenylethylacetate normally congeal and form lumpy masses α-Pinene Phenylethylalcohol under steam distillation, where steam would not penetrate, like rose petals and Sabinene orange blossoms. This method is also Terpinen-4-ol useful for fruit kernels that would form α-Terpineol glutinous masses under steam distillation Terpinolene and powdered forms of plant material July 2012 P E R S O N A L C A R E 69
  • 4. ESSENTIAL OILS slightly less than the boiling point of water, the plant surface material as possible material from directly coming into contact due to the mixed liquid of solublised during the distillation. with the heating coils. volatiles and water. Heat applied to the still The effects of hydro-diffusion are much With many materials, part of the oil will cause the creation of a small bubble of slower in water than other types of dissolves in the water during distillation and saturated mixed vapour from the liquid distillation. Consequently, especially for forms a milky emulsion, as a number of phase, where upon formation it rises to the wood materials extensive comminution aromatic constituents are soluble to some top of the water in the charge. During the must be undertaken so that particles in the degree in water. This loss could range up to rise, the bubble’s pressure, temperature charge are fine and as much oil as possible 25% of the essential oil.7 This means that and proportion of oil to water decreases. is exposed on the surface of the material. the recovery of oil is incomplete and the The condensing volatiles, mostly being less In water distillation, plant material is recovered oil will be deficient in some dense than water, float to the top of the placed in a sealed vessel or retort that constituents that would be the case with water and form a film on the surface of the connects directly to a condenser. From the the oil recovered through steam distillation. water in the vessel. This lost oil tends to condenser the distillate runs into a Upon separation in water distillation, the remain on top of the surface and cannot separator. The rate of distillation is water distillate is returned directly to the re-vaporise easily due to its higher boiling controlled by the intensity of the fire, the charge vessel to replace the decreasing point and the generally cooler temperatures pressure of the vessel or retort and/or the water level due to evaporation. This is at the water surface. Most of the oil rate of introduction of steam. As many called cohobation. Sometimes the water recovered in water distillation is the portion woods contain high boiling compounds, distillate is redistilled in another vessel to of the oil that does not condensate through pressure is vital to create high enough extract the volatiles in emulsion. Salt is this action. temperatures to vaporise the volatile often added to the distillate to reduce the Observation shows that distillation constituents. These constituents may take solubility of water. Whether this process is undertaken with vigorous boiling produces many hours to boil out. Hydro-stills should undertaken depends upon the probability of better and quicker yields than mild boiling. generally be wide to maximise the the constituents being damaged by further Some distillers even install small propellers evaporation area. Where particles are fine heat and the economics of re-distillation. intruding into the side of the still to assist such as saw dust and powders some form Another method to recover the dissolved in agitation. This is most probably effective of mesh or “P” shape pipe arrangement aromatic materials from the water distillate because the agitation in the charge tank should exist at the entrance to the is to add a solvent. The mixture is then prevents oil droplets clinging to the herb condenser to prevent plant material from vigorously shaken to pick up dissolved surfaces. It is necessary to generate entry and possible clogging. Heavy charges constituents from the water into the enough steam in the water so that it will and where heat coils are used in the still solvent. These materials are then recovered come in contact with as much of the oil on require a perforated grid to prevent plant through vacuum distillation of the solvent Table 2: A comparison between water, water and steam and steam distillation. Water distillation Water and steam distillation Steam distillation Construction Usually simply constructed, Inside vat contains a grill where Utilises an outside steam source based on ancient designs. plant material rests above the water Plant material suitability Finely powdered materials such Can be used for most herb and Most materials, except fine as woods and rhizomes, flowers leaf materials. Material must powders. Good for high boiling that congeal with steam. be packed in a uniform materials. Material must be packed Not suitable for materials that manner to avoid channeling in a uniform manner to contain acidic material which can of steam. avoid channeling of steam. saponify, water soluble or high boiling constituents. Material must be completely covered with water. Hydro-diffusion Excellent Good Steam should be slightly wet to promote diffusion. Superheated or high pressure steam can dry out the plant material and inhibit diffusion. Available Pressure Atmospheric pressure Atmospheric pressure Can be adjusted for both high and reduced pressures. Available Temperature 100˚C, but care must be taken Approximately 100˚C Can be increased or reduced not to burn the plant material according to pressure used. from direct heat on the sides. Hydrolysis Condition Usually a high rate of ester Hydrolysis is usually low, however Slight hydrolysis. hydrolysis. excessive wetting of the plant material through prolonged distillation can promote hydrolysis during later stages of distillation. Rate of distillation and yield Slow rate of distillation. Moderate distillation rate. Fast rate of distillation. Low rates of yield due to Good yields if no channels Good yields if no channels hydrolysis and loss of water occur in charge. Usually good yields. occur in charge. Usually good yields. soluble constituents into the water. High boiling constituents often left undistilled. 70 P E R S O N A L C A R E July 2012
  • 5. ESSENTIAL OILS which results in a secondary essential oil.8 Some common water soluble aroma chemicals in essential oils are listed in Table 1. Another method that will contribute to minimising oil loss due to oil solubility in water during the separation phase is to control the outgoing distillate temperature from the condenser. Where oils are less dense than water, there will be an optimal temperature range where oil particles will freely float to the top of the distillate upon condensation. Some literature on distillation practices misses the point about the effect of condensation temperatures on oil yields.9 Based on private work,10 the higher the temperature of the outgoing distillate, the freer will be the oil particles to float to the top. For example, tea tree oil droplets will float to the top of the water distillate twice as fast at 60°C than at 40°C. The upper temperature limit will be restricted by the potential loss of low boiling volatiles during condensation. This has implications on the design of the Figure 4: The condenser, with the end manifold removed to expose the internal cooling pipes, specific condenser for specific crops and at the author’s property in Perlis, Malaysia. set range limits upon the temperature that distillation can take place, to achieve a water distillation. Water and steam steam distillation facilities are designed and specific outgoing distillate temperature distillation has another advantage over built with the correct steam ratings, they range. steam distillation as there are fewer are much more economical to run than decomposed products during the process water and water and steam distillation Water and steam distillation due to less chance of plant material drying systems. A comparison between water, Water and steam distillation involves the out. However water and steam distillation water and steam and steam distillation is storing of the plant material above a water will take a lot longer. Water and steam shown in Table 2. below. bath situated in the bottom of the charge distillation can produce very good results vessel and heating the water either through under reduced pressure. The condenser system direct fire, a steam jacket or a closed or Water and steam distillation is much A condenser in an essential oil distillation open steam coil. Water and steam cheaper to set up than steam distillation system is a heat exchange or dissipating distillation produces saturated wet steam at facilities and lends itself to portable stills device. The condenser must not only cool the prevailing vessel pressure, which is that can be transported from place to the condensate vapour into a liquid, but usually atmospheric pressure. Within this place. also cool the condensate to the configuration, unlike water distillation, only temperature range where the oil will steam comes in contact with the plant Steam distillation separate spontaneously from the water. material. Steam distillation employs an external The usual array for a condenser system Water and steam distillation is not very steam generation system, external to the is a tube or set of tubes running through a suitable for fine materials as steam will find charge vessel. This configuration provides sealed water reservoir to cool the pipes. It a path of least resistance tending to create much more control (depending upon the is immediately attached to the top of the channels. This means that steam will not boiler capacity) than water and steam charge vessel to collect all vapour exiting flow through the whole mass of plant distillation. This is because in steam the vessel. The design of the condenser material and an incomplete distillation will distillation the wetness fraction, must ensure that the vapour flow is take place. If the plant material is loosely temperature and pressure can be turbulent inside the tubes to prevent high packed, the same effect will happen, as manipulated according to needs and velocity vapour freely flowing through the the material will offer no resistance to the conditions. However, it is a misconception condenser and maximise exposure to the steam. that greater steam volumes and increased cooler walls. A baffle is usually installed at Water and steam distillation may take a pressures have positive effects on the the beginning of the condenser to disrupt a long period of time to reach operating process in all cases. As mentioned straight steam flow for this purpose. Failure temperature as the plant material needs to previously, dry and superheated steam has to achieve those conditions would result in be heated up with only saturated steam. the effect of drying out plant material, some vapour failing to condensate. Within This may cause early condensation and which potentially halts distillation through the condenser system the flows of vapour wetting of the plant material. the stopping of hydro-diffusion process. and cooling water should be in opposite Due to the limits on pressure that can Faster steam flow rates do not necessary directions at the maximum possible speed. be built up in the charge vessel, water and mean quicker recovery times. Fabricated The condenser must be sensitive enough to steam distillation will have only a limited steam boilers cost much more to run than react on the vapour flow very quickly. The effect on extracting high boiling materials water baths and may lead to high required number of tubes and length of the from plant materials. However there is less distillation costs, especially if they require condenser depends on the rate of distillate opportunity for hydrolysis to occur than with petrochemical feed stocks. However if flow, the pressure, the temperature of the July 2012 P E R S O N A L C A R E 71
  • 6. ESSENTIAL OILS cooling water and the desired exit microscopic oil droplets. Temperature plays Distillate in-flow from still temperature range of the distillate. (water-oil mixture) a crucial role in separation, where it should The condenser must remove the be moderately warm to increase the equivalent amount of heat that is needed relative specific gravity differential of the oil to vaporise the distillate, plus the additional Oil and water. Raised temperature of the outlet amount of heat to reach the optimal distillate water will allow the small oil distillate temperature range of the particles to rise to the top of the separator condensate distillate exiting the condenser. quicker in a similar manner to the The rate of which heat would be removed condenser exit temperature range where from the distillate can be represented by Water there will be an optimal separator water Internal outlet the following equation: baffle temperature range to promote oil-water Q = UA∆t ∆ separation.11 Where Q = the heat removed by unit During distillation, the more volatile of time constituents tend to vaporise quicker and U = a constant determined by the less volatile constituents vaporise later operating conditions (condensing and in the distillation. This leads to an oil that cooling made up of a number of will vary in constituents during the factors) usually a constant is used. distillation period. By changing separation A = the area available for heat flasks at particular points during a single removal distillation, oils of different constituent ∆t = the temperature difference profiles can be collected. This is important between the vapour and the cooling Figure 5: Schematic view of a hydro-diffusion in ylang ylang and lavender distillation, medium. distillation system. where different oils profiles will have different uses and values to particular U is made up of a number of factors possible separate the oil from the distillate customers. Many distillers also use this including the flow rates of cooling water water. As distillate water volume is much principal to collect specific fractions during and vapours, the material that the greater than oil, it is important that water the distillation, which can later be blended condenser is constructed, and usually a can be removed continuously. Oil and together to create a whole oil that meets constant is used due to the difficulty to water separates according to specific with certain specific specifications, such as calculate. The value of U increases as gravity forming two layers. Lighter than a standard. these factors increase. Thus according to water oils will float to the top and heavier The water distillate will always be the equation, the surface area can be as than water oils will sink to the bottom. This saturated in oil and directly dumping it large or small as desired, as long as the must be considered in separator design for would lead to a loss in yield. For this other factors compensate. However the water removal. reason some distillers (water and water and overall capacity of the distillation system If the specific gravity of oil and water is steam distillation) will channel the water will have great bearing on the condenser very close, the two components will not distillate back into the still vessel for re- area. Condenser sizes will also vary in size separate immediately. Distillate flowing into distillation in what is called cohobation, according to the temperature of available the separator must therefore not disturb mentioned previously. For this purpose the cooling water on site, thus condensers in the surface area and flow into the body of separator must be placed higher than the temperate and tropical areas will reflect the water to prevent surface turbulence. still vessel proper so distillate water in the this in size. The separator must also be large enough separator can be fed back into the still Using a condenser system with the so that drained water does not carry away through gravity. wrong capacity for the distillation system will have a number of operational Steam inlet consequences. A too efficient condenser system will deliver the distillate at a temperature below the optimum range, which could lead to cool air outside being Downward steam flow sucked into the system. This outside cooler air in the condenser tubes could create expansion and contraction of vapours in Plant material the condenser leading to splattering and Side opens so that intermittent distillate outflow. This could cartridge with plant also occur if the cooling water is too cold. material can slide in Grated base If the condenser is too small for the and out of still distillation system, then the still must be operated with lower steam rates, which Condenser array would lengthen distillation times and open up the possibility of hydrolysis to occur within the vessel. Water and oil collector The separator system Before leaving the subject of distillation in this chapter, some words about the Collector vessel separator system must be mentioned. The function of the separator is to as quickly as Figure 6: Oil separator design used in Perlis, Malaysia. 72 P E R S O N A L C A R E July 2012
  • 7. ESSENTIAL OILS Hydro-diffusion material near the bottom may also lead to 6 Guenther E.The Essential Oils, Volume One: distillation hydrolysis and lead to lesser yields. History – Origin in Plants, Introduction – Analysis, Hydro-diffusion distillation is a variation on However, hydro-diffusion distillation appears Malabar, Florida, Robert E. Krieger Publishing steam distillation where steam is popular within the aromatherapy industry in Company, P 110, 1948. . introduced on the top of the vessel and Europe. PC 7 Fleisher A. Water-soluble fractions of the condenses through the plant material in essential oils, Perfumer & Flavorist 1991; the still, where the distillate is collected ɀ The final article in September will 16 (3): 37-41. and condensed under the plant material conclude with a brief discussion about 8 Bouzid N, Toulgouate K, Villarem G, Gaset A. which rests on a grill or perforated tray. applying these principles. Analyse quantitative des fractions d’huile Through steam travelling down the still, essentielle pouvant co-exister lors there is more time for the volatiles and References d’hydrodistillation de plants aromatiques, fatty acids floating on the plant material. 1 Johannes AK, Scheffer JC, Svendsen AB. Rivista Ital Eppos 1997; 79: 15-25. In the case of wood and seeds that have Comparison of Isolation Procedures for Essential 9 Boland DJ, Brophy JJ, House APN. Eucalyptus many high boiling compounds, which are Oils, Z. Lebensm. Unters. Forsch, Vol. 168, Leaf Oils: Use, Chemistry, Distillation and difficult to vaporize in an ordinary still, this 1979, pp. 106-111. Marketing 1991; Melbourne, Inkata Press, P . system may be effective. This would be 2 Private communication with Mr. Jon Bonnardeaux 191. valuable when fatty acids contribute to the of Western Australia Department of Agriculture, 10 Unpublished private work on tea tree distillation flavour of a material and it is desirable in early 1990s. at Batu 9, Berseri, Perlis, Malaysia during the oil. Thus, hydro-diffusion distillation 3 Denny EFK. Field Distillation for Herbaceous Oils, 2004/5. may return an oil more representative of Lilydale, Tasmania, Denny McKenzie & 11 Hughes AD, (1952), Improvements in the Field the plant’s natural profile.12 Associates, P 81, 1990. . Distillation of Peppermint Oil, Corvallis, It is reported that hydro-diffusion 4 Kristiawan M, Sobolik V, Al-Haddad M, Allaf K. Engineering Experimental Station Bulletin No. 31 distillation gives quicker distillations with Effect of pressure drop on the isolation of 1952; Oregon State College, 1-64. lower steam consumption than cananga oil using controlled pressure drop 12 Legast E, Peyron L. Hydrodiffusion Industrial conventional steam distillation.13 However process, Chemical Engineering and Processing Technology to Produce Essential Oils by this process is governed by the physical 2008; 47 (1): 66-75. Steam, in Proceedings of the 11th International laws that govern any other type of 5 Rezzoug SA, Boutekedjiret C, Allaf K. Congress of Essential Oils, Fragrances distillation and the fact that the steam Optimization of operating conditions of rosemary and Flavors Vol. 2 1989; New Dehli, India, travels downwards while cooling may affect essential oil extraction by a fast controlled 69-73. the transfer of latent heat and thus pressure drop using response surface 13 Hall R, Klemme D, Nienhaus J. The H&R Book: increase, rather than decrease distillation methodology, Journal of Food Engineering 2005; Guide to Fragrance Ingredients Vol. 4 1985 time. The tendency to saturate the plant 71 (1): 9-17. London, Johnson Publications, P 13. 0 . July 2012 P E R S O N A L C A R E 73