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Murray Hunter – University Malaysia Perlis            ESSENTIAL OILS




                             The distillation of
                              essential oils 3:                                                             PART


      The final part of this series on distillation carries on from the basic principles, stages and types of distillation
             to look at harvesting, selection and design of a distillation system, and the scaling up process.

Harvesting                                                                                                       However under plantation
The method and timing of                                                                                         cultivation, the whole tree is
harvesting crops will depend                                                                                     coppiced at an early stage,
upon the part of the plant                                                                                       where it will usually re-grow
required, the pre-processing                                                                                     increasing leaf biomass for
preparation required before                                                                                      future harvests. This is also the
extraction, the re-growth                                                                                        case with tea tree (Melaleuca
characteristics of the crop,                                                                                     alternifolia) where initial growth
the changes of chemical                                                                                          from a seedling will have a
constituents in the plant during                                                                                 singular trunk where coppicing
growth, the diurnal variance of                                                                                  after the first year and breaking
chemical constituents in the                                                                                     up the trunk butt at ground
plant, the characteristics of the                                                                                level, will promote multiple
field and the type of enterprise                                                                                 stem re-growth, promoting
in terms of size, scale and                                                                                      more biomass (Fig. 1). Table 1
socio-economic environment                                                                                       shows the length of the first
it operates within.                   Figure 1: Broken up tea tree trunk to promote coppice growth.              harvest time from planting
    As essential oils can be                                                                                     and method of harvest.
sourced from leaves, stems, flowers, bark,       combing them from branches in some                   Some crops like peppermint have a
wood, fruits, rhizomes or seeds, the nature instances.                                             distinct harvest window where phyto-
of the plant material required will have             With trees like eucalyptus and lemon          chemicals within the leaves synthesise and
great bearing on the mode of harvesting          myrtle, a portion of the leaves are usually       convert into desirable constituents that
required.                                        lopped off for distillation, leaving the bulk     give the oil its commercial value. These
    Flowers are more delicate than other         of the tree intact for growth. These trees,       processes depend upon seasonal factors
plant tissues and mechanisation may              if mature in the wild, will have difficulty       and temperature conditions, i.e., in the
damage them. Thus many flowers like              re-growing if completely chopped down.            case of peppermint daylight hours and
rose and cananga must be picked
manually. Some jasmine and boronia are
mechanically harvested through combing                                      Optimum harvest window
                                                      80                                                                                      80
arrays, although the effectiveness of this
is unknown. Bark can be scraped off from              70                                                                                      70
trees or collected as a by-product of the
timber industry. However many bark                    60                                                Oil yield                             60
products come from remote areas in
                                                                                                                                                Yield (kg/ha




tropical countries and are still collected            50                                                                                      50
                                                   % in oil




manually by collectors from both the wild
and plantations. Woods have to be cut in a            40                                                                                      40
                                                                                                                     Menthol
similar manner to how the timber industry
                                                      30                                                                                      30
would harvest a tree. Fruits are usually
utilised for other products like citrus juices,                                                          Menthone
                                                      20                                                                                      20
and the peels which contain oil are
processed as a by-product. Rhizomes must              10     Methyl acetate                                                                   10
be collected from underground, either                                                                       Menthofuran
manually or through mechanical upturning                  1      2      3      4      5      6    7      8       9      10       11     12
of the earth. Seeds are either directly                                                 Weeks from 1 January
collected from the ground or plant when
mature via manual or mechanically                Figure 2: The harvest window applicable to the Victorian and Tasmanian mint industries.

                                                                                                    September 2012 P E R S O N A L C A R E                 1
ESSENTIAL OILS


night time temperatures. Plants like
Artemisia vulgaris change in constituent
levels throughout their growth cycle, so it is
important to determine the optimal harvest
time based on maturity.1 Determining the
optimal harvest time requires sampling and
graphing of the leaf oil constituents over
the crop lifecycle. Figure 2 shows the
harvest window applicable to the Victorian
and Tasmania mint industry in Australia.2
    Some flowers exhibit diurnal variations
in constituents and the daily timing of
harvest is critical. This is the case for
rose and jasmine which may have to be
harvested in the very early hours of the
morning to obtain the optimum
constituents in the flowers for extraction.
Other flowers where this issue is important
include Hoya carnosa, Stephanotis
floribunda,3 Syringa vulgaris,4 Narcissus
tazetta and Osmanthus fragrans.5
    Harvesting methods and timing are                  Figure 3: Paddle arrangement connected to tractor wheel for ‘boggy’ conditions


    Table 1: The length of harvest time and method of harvest for some essential oil crops.

    Common name                 Time from initial planting to first harvest       Method of harvesting
    Australian Tea Tree         Usually can make first harvest 8-12 months        Usually mechanised harvesting where the whole tree is cut and
    Melaleuca alternifolia      after planting. Second and subsequent             mulched for easy distillation. First harvest tree will be a single trunk,
                                harvest every 6-13 months, depending              but after harvest stump is smashed so tree can coppice many trunks.
                                upon climate.                                     Manual harvest is undertaken in Malaysia, Cambodia, etc.
    Basil, Ocimum basilicum     Plants usually flower at 50-60 cm height          Plants are cut immediately upon flowering, either manually or
    and sub-species.            after 3-6 months.                                 mechanically. Basil should be replanted after harvest.
    Black Pepper,                                                                 Harvested when plants fruit, just when they start to ripen.
    Piper nigrum                                                                  This is usually a manual operation and occurs several times
                                                                                  during the season.
    Calamus Oil,                Usually can be harvested 6-10 months after        Rhizomes must be dug up by spade or plough, washed and dried before
    Acorus calamus              planting                                          distillation.
    Cananga/Ylang Ylang         Usually in 2nd year, peak after 5th year.         Manual picking: Flowers should be picked when early in the morning to
    Cananga odoratum                                                              maximise oil content, only after they have turned yellow. Ropes are
                                                                                  sometimes attached to the branches so pickers can pull them down to
                                                                                  pick off the flowers without having to climb the tree.
    Cassia Bark, various        Cinnamomum cassia: First harvest approximately    Cinnamomum cassia: Trees coppiced and pruned by hand to strip leaves
    Cinnamomum species          5-7 years when trees coppiced at 3 m height.      and bark for oil production.
                                Cinnamomum verum: first harvest 2-3 years         Cinnamomum verum: Tree coppiced at 3 m height after 2 years for
                                after planting                                    bark by hand.
    Citronella, Cymbopogon      Usually first harvest can be undertaken between   Small holders will manually harvest with a sickle and carry to the
    nardus                      4-5 months after initial planting, with           still for distillation. Foliage harvesters are used on larger fields, which
                                subsequent harvests every 3-4 months.             chop and collect the material. Most oil is in the leaves so cutting
                                                                                  distance set to where the bulk of the leaves are (18-28 cm).
                                                                                  This also allows faster regrowth. Crop can have a commercial life of
                                                                                  4-10 years.
    Coriander seed,             Usually after 6 months with coordinated spring    When the plant is 50-70 cm in height and fruit is 5-7 mm in size
    Coriandrum sativum          planting and autumn harvest.
    Geranium, many species      Crop usually grows enough foliage for first       Usually mowed around 10-15 cm above the ground as little oil in the
    and hybrids of              harvesting 6-9 months after planting              stems [143] and to allow for re-growth.
    Pelargonium
    Ginger, Zingiber officinale Harvest can occur anywhere between 150-300 It is important to determine the optimal level of oil and oleoresin content
    and other species           days after planting, depending upon temperature in the rhizomes before harvesting. Harvesting can be manual or
                                conditions.                                     mechanised, as whole plant is pulled out, which must be without
                                                                                damage.
    Jasmine, various            Jasmine may take 4-5 years before productive.     In warm humid areas, flowers can be continually harvested for around
    Jasminum species.                                                             6-9 months per year. Flowers should be picked before sun rises 20%
                                                                                  above the horizon and a daily basis to avoid loss of volatiles. This is a
                                                                                  manually process, although combing and suction systems have been
                                                                                  experimented with. Plants are usually pruned after each flowering
                                                                                  season to promote growth.


2        P E R S O N A L C A R E September 2012
ESSENTIAL OILS


affected by the physical state of the              as is in the case of patchouli where it must           the tyres of the harvesting equipment, so
fields. Hilly fields restrict the degree of        be stored before distillation.                         that the crop can be effectively harvested.
mechanisation during harvesting,                       An important consideration in the design               Planning of the harvest is of paramount
particularly if the gradients are high.            of any harvesting system is the potential              importance as it must be synchronised with
The weather, particularly rain, will degrade       damage on the plant material. Some plant               the capacity of the distillery to ensure there
field compactness and can lead to delays           material is very easily bruised or damaged,            is no undesired backlog of unprocessed
in harvesting as conventional harvest              which would restrict mechanisation options.            material waiting to be distilled. Ideally,
equipment may have trouble operating on            This is why some traditional harvesting                harvest should be followed by almost
waterlogged fields, particularly in tropical       methods are still widely used for a number             immediate distillation, where appropriate.
areas. Mechanised harvesting equipment             of essential oil crops.                                The distance of the field from the distillery
can be adapted to waterlogged fields                   The most efficient method of harvesting            is also a consideration and harvest times
through paddle arrangements connected              is to cut the material in the field and load           over a diverse region utilising a central
to the wheels of tractors and bins.                it directly into a container that will also act        facility, requires very careful logistical
This method is successfully used in rice           as the charge vessel during distillation. This         planning. Where crops like mint require
paddies throughout South-East Asia.                causes some loss of oil and inefficiency in            some time to wilt after being mowed before
    The harvesting system should ideally           yields due to non oil-bearing plant material           being picked up by a forage harvester and
be integrated with the extraction system           also being harvested, i.e., twigs and                  deposited into buns, delays in the two
for maximum efficiency. This is restricted         branches in tree crops. But overall this               operations can lead to excessive wilting,
by any pre-extraction wilting and/or               is much more economic than selective                   which will greatly reduce oil yields. Wilting
comminution required before extraction,            harvesting of plant parts. If crops are                times may be heavily influenced by daily
as any pre-processes increase the time             mechanically harvested, row planting must              wind and temperature conditions, requiring
lag between harvest and extraction, such           be coordinated with the distance between               great flexibility in the time lag between


 Table 1 (continued): The length of harvest time and method of harvest for some essential oil crops.

 Common name                Time from initial planting to first harvest         Method of harvesting
 Lemon scented gum,         First harvest 6-12 months after planting.           If grown solely for oil production, trees should be regularly topped and
 Eucalyptus citriodora      After 2nd year tree can be felled for re-growth.    coppiced to maintain growth. A height of around 2.5 m maintained.
                                                                                Alternatively trees can be felled, leaving the main stem for re-growth of a
                                                                                coppice of young shoots, which can be re-harvested every 6-12 months.
 Lemon Scented Tea          First harvest after 2-3 years, subsequent           A foliage harvester can coppice the tree when re-growth warrants it.
 Tree, Leptospermum         harvests each year.
 petersonii
 Lemongrass,                Usually first harvest can be undertaken between Small holders will manually harvest with a sickle and carry to the still for
 Cymbopogon flexuosus       4-7 months after initial planting with subsequent distillation. Foliage harvesters are used on larger fields, which chop and
                            harvests every 3-5 months.                        collect the material. Most oil is in the leaves so cutting distance set to
                                                                              where the bulk of the leaves are (15-20 cm). This also allows faster
                                                                              regrowth. Crop can have a commercial life of 4-5 years.
 Nutmeg, Myristica          Trees from seed bear fruit between 6-10 years,      Fruit is allowed to split and either picked or allowed to fall to the ground
 fragrans                   vegetative propagated trees 5-7 years.              and collected on a daily basis. Nets can also be used to catch the
                            Fruit ripens around 6-9 months after flowering.     falling fruits. Long poles with cutters also used.
                            Reach maximum yields after 20 years.
 Palmarosa, Cymbopogon      First harvest around 6 months after planting        Plants should be mechanically or manually harvested about 10 cm from
 martini var. motia         Further harvests when flowering occurs every        the ground, when flowering begins, around 6 months after planting.
 and sofia.                 6 months.
 Patchouli, Pogostemon      Can be harvested 4-8 months after planting          Usually the leaves are cut manually or mechanically, dried and stored to
 cablin                     and subsequent harvests at 3-6 month                allow some fermentation, before distillation at a later time.
                            intervals for a 2 to 6 year period.
 Peppermint, Mentha         Planted in early spring and harvested mid to        The crop is usually mowed, allowed to wilt and them scooped up into
 piperita                   late summer.                                        bins for distillation. This is usually an automated process.
 Rose, Rosa species                                                             Flowers picked manually between 5-10 am in the morning,
 (usually R. centifolia                                                         while flowers still open.
 and damascena)
 Sage, Salvia officinalis   Trees can be trimmed after first year for           Trees can be trimmed for leaves each year and dried.
                            around 6 years.
 Sandalwood, Santalum       30-50 years after planting                          The oil is contained primarily in the heartwood and large roots, thus the
 album and S. spicatum                                                          tree must be felled and pulverized.
 Tasmanian Blue Gum,        Trees can be lopped after 6-12 months, upon         Trees either coppiced and lopped when dedicated to oil production
 Eucalyptus globulus        reaching around 3 m height. Trees then allowed      manually or through mechanized lopper. If trees cultivated for timber,
                            to coppice for lopping and coppicing every          harvest after tree felled around 5-8 years of age.
                            9-15 months.
 Vertivert, Vetiveria       First harvest usually 18 months after planting to   Usually the foliage is cut and slashed prior to the lifting of rhizomes
 zizanioides                allow rhizomes time to mature.                      (sometimes burning used). Roots either dug up manually or dug up with
                                                                                the aid of a mechanical digger. As much vetiver is planted on hill slopes,
                                                                                harvesting is a very difficult process to mechanise.



                                                                                                          September 2012 P E R S O N A L C A R E               3
ESSENTIAL OILS


mowing and picking up the foliage for                 ɀ Efficient collection of the material in the    these systems will fulfill their requirements.
distillation.                                           field and delivery to the distillery.          Fabricated ‘turnkey systems’ are offered by
    Still today a large amount of harvesting          ɀ Minimisation of backlogs in material to        some suppliers, however, they account only
is undertaken either manually as is the                 be distilled, and                              for a small percentage of actual working
case in Indonesia, Cambodia and Vietnam               ɀ Minimal delays in harvest to distillation      field stills in the industry. Most stills are
by small holders. ‘Outback’ stills are still            times, according to requirements.              locally fabricated with local materials taking
used in Australia for tea tree, where the                                                              advantage of the local topography and
farmer collects wild or small scale                   Selection and design                             energy sources, usually fitting in with the
plantation material with a tractor and                of extraction system                             socio-cultural way cultivation is undertaken
trailer, to be loaded into the still upon             The choice of method for essential oil           in their geographical location. This would
returning from the field. Although some               extraction will depend upon:                     include the majority of small holder
companies offer state of the art harvesting           ɀ The sensitivity of the aromatic                production, cultivating small plots or
equipment, many producers fabricate their                constituents in the plant to heat.            collecting from the wild in Indonesia and
own specialised equipment, utilising                  ɀ The sensitivity of the aromatic                Vietnam. Similarly, boutique farms
standard agricultural machinery available.               constituents in the plant to moisture.        producing specialty essential oils like
Over a period of years during the winter              ɀ The volatility of various constituents         lavender, tea tree, manuka and lemon
months, this equipment is rebuilt and                    within the plant.                             myrtle in Australia and New Zealand would
modified to suit their small to medium                ɀ The physical nature of the plant tissue.       also in the majority of cases employ simple
scale operations. Large scale operations in           ɀ The solubility in water of the aromatic        designs. Only large extensive farms
the mint, citrus, eucalyptus and tea tree                constituents within the plant.                producing large tonnage oil like mint and
industries utilise equipment that brings the                                                           the larger Australian tea tree plantations
most efficiency to the operation, as a low            An overview of some of the issues involved       would develop capital intensive ‘integrated
production cost is of great importance to             in selecting an extraction process can be        production systems’.
survival.                                             seen in Figure 4.                                    A number of factors must be taken into
    Good management of the harvesting                     A summary of the extraction methods          consideration when designing a distillation
procedure requires:                                   used for a number of essential oils is listed    system for the project:
ɀ The determination of the optimal harvest            in Table 2.
    time.                                                 The comments in the rest of this             The nature of the plant material
ɀ Precise mowing or harvesting of the                 section are primarily related to distillation.   This would lead to considerations such as;
    herb with minimal damage to the crop.             A great number of distilleries tend to be        what are the absorption characteristics of
ɀ Consistent and precise wilting, if                  locally built and designed from what             the material? What would the most
    required before extraction.                       information people have in the hope that         important distillation fundamentals that

    Table 2: Methods of extraction utilised for a number of essential oils.

    Essential oil         Botanical name                             Part of plant used for extraction Usual method(s) of extraction
    Star anise oil        Illicium verum                             Seeds                             Steam distillation after seeds are comminuted
    Artemisia oil         Artemisia vulgaris                         All the herb                      Steam distilled after drying
    Basil oil             Ocimum basilicum                           All the herb                      Steam distilled after drying
    Bergamot oil          Citrus bergamia                            Fruit Peels                       Cold expression of nearly ripe fruits
    Broom absolute        Spartium junceum                           Flower blossoms                   Solvent extraction
    Cajuput oil           Various Melaleuca species                  Leaves and twigs                  Steam distillation of fresh material
    Calamus oil           Acorus calamus                             Roots                             Steam distillation of fresh or dried material
    Cananga oil           Cananga odorata                            Flowers                           Steam distillation of fresh material
    Cedarwood oil         Juniperus virginiana                       Wood chips, sawdust               Steam distillation
    Celery Seed oil       Apium graveolens                           Seeds                             Steam distillation of crushed seeds
    Citronella oil        Cymbopogon nardus                          Grass                             Steam distillation of dried material
    Coriander seed oil    Coriandrum sativum                         Seeds                             Steam distillation fo crushed dried seeds
    Fennel oil            Foeniculum vulgarie                        Seeds (in fruits)                 Steam distillation of the crushed seeds
    Ginger oil            Zingiber officinale                        Rhizomes                          Steam distillation of freshly ground rhizomes
    Jasmine absolute      Jasminum grandifloram and other            Flowers                           Solvent extraction of the fresh flowers
    Lavender oil          Lavandula officinalis and others           Flowering tops and stalks         Steam distillation of fresh material
    Lemon oil             Citrus medica                              Peel                              Cold expression
    Lemongrass oil        Cymbopogon flexuous and citratus           Grass                             Steam distillation of fresh or mildly wilted grass
    Lime oil              Citrus aurantifolia                        Peels                             Steam distilled or cold pressing
    Litsea Cubeba oil     Litsea cubeba tree                         Ripe fruit                        Steam distillation
    Patchouli oil         Pogostemon cablin                          Leaves                            Steam distillation of dried and fermented
                                                                                                       leaves under pressure
    Rose oil              Rosa centifolia, damascena and others      Flowers                           Water distillation of fresh flowers
    Sandalwood oil        Santalum album                             Wood                              Steam distillation of chipped and powdered wood
    Thyme oil             Thymus vulgaris                            Flowering herb                    Steam distillation



4        P E R S O N A L C A R E September 2012
ESSENTIAL OILS


would apply to this material? What would
be the effect of steam and/or water on the
physical state of the material (i.e., will it
congeal or tend to form steam channels)?
Will the material have to be pre-processed
before distillation (i.e., cut up, ground or               Influencing Factors                                                       Historical
some other form of comminution)?. Is the                        Compound
                                                             characteristics
material sensitive to delay in distillation?             (volatility/mol. Weight)
Does it have to be wilted? Are the volatile               Surrounding Material                                    Compounds          Highly volatile
                                                                                                                  mixed with           terpenes
constituents subject to damage at                                                                                 waxes, also
prolonged high temperatures? Are there                                                                            lactones,
                                                          Low/medium volatility/stable
                                                                                                                  esters etc.
low and high boiling constituents?
What considerations must be given to this?                                   Distillation                 Solvent                     Cold
How do others distill this material?                                                                     Extraction                 Pressing
    These questions would assist in
identifying the most suitable type of
                                                                                                                                     Automated
distillation method and the general                                                                                                  harvest and
practices that will be applied during                     Influencing Factors                             Harvest and
                                                                                                                                      distillation
                                                            Price vis. Market                          later load system               system
distillation, such as what type of steam,                         Volume
for how long should it be distilled, etc.                Plant cell structures
                                                                 Field size
                                                                Topography
The harvest method and logistics                        Soil/field characteristics
The harvest methods used will depend                       Part of plant (i.e.,                                                        Extensive
                                                               rhizome/leaf)                     Manual                               large scale
upon the scale of the project, the nature of
                                                                 Coppice                                          High --- Low
                                                                                                harvesting                              farming
the herb, the local traditions and practices                                                                         Value
                                                                                                  due to
of farming, the capital investment made                                                           scale,
into the venture and the amount of the                                                           material,                      Specialties
                                                           Distillation                        investment
particular herb that requires handling and
processing. Harvest methods can vary from
manual harvesting, mowing and wilting
                                                                Hydro                 Material
before being picked up from the field by                                            Characteristics                                   ‘Finer’
another vehicle, to a fully integrated system                                                                   CO2                 composition
                                                                                                                                     spectrum
where the material is harvesting, mulched                                            Solubility in
                                                           Water-Steam
and spread directly into a cartridge or box                                            water
                                                                                                                                      Individual
array, behind the tractor/harvester. Another                                                                 Fractional
                                                                                                                                        aroma
                                                                                                             Distillation
consideration is the potential damage that                                                                                           compounds
could occur to the plant material through                      Steam                  Material
                                                                                    Characteristics
harvesting, as in the example of rose petals
which must be picked by hand to prevent                       A Basic Harvest to Distillation Flowchart for
any damage which could promote                                                        Peppermint Oil
                                                   Figure 4: Some of the factors influencing the mode of extraction of essential oils from plants.
hydrolysis, oxidation and resinisation before
distillation. Time between harvest and
distillation is another factor that needs                  Determination of Harvest time
                                                                   (Sampling)
consideration. In the case of rose petals,
distillation time after harvest is very crucial,
where time is not as critical for eucalyptus                                                                      10 tonne fresh herb per Ha.
                                                            Mowing and leaving to wilt on
and tea tree oil distillation. Basically a                             field                                      Fresh herb contains 80%
‘time and motion’ flowchart of the logistical                                                                     moisture

aspect of harvest to distillation can
be undertaken, which can assist in                                         Wilting                                Must wilt to 50% moisture
determining the amount of integration                                                                             level where ‘crisp and
                                                                                                                  brittle’
between harvesting and distillation
systems. This needs to be quantified with
                                                            Pick up with forage harvester
expected volumes on a daily basis to assist                                                                       Collect 6 tonne of dry herb
in determining the required still capacity,
steam requirements and overall still design.
                                                                                                                  Must insure that herb is not
A flowchart for mint is shown in Figure 5.                  Deliver to Distillation system                        bruised.
                                                                                                                  Use cartridge or box to
                                                                                                                  avoid too much handling
Available cooling water for condenser                                                                             Volume of 4 M2 per tonne
An important factor in condenser design is                                                                        of herb.
                                                                        Distillation
the temperature of the available water                                                                            If single charge, yield 15kg
                                                                                                                  oil
for cooling. This will greatly influence the          Assume 35 minutes distillation time, 10
size of the condenser along with vapour               minutes change over, 6.90 litres/minute                     If distillate ratio is 0.062/1
                                                      steam rate per minute. 9 hours will handle                  (oil/water), then 241.8 litres
throughput. Ignoring the condensate water             12 tonnes of dried herb in a vat of 4m 3.                   water required for
                                                                                                                  distillation.
temperature issue when designing the
condenser could lead to expensive re-              Figure 5: A basic harvest to distillation flowchart for peppermint oil.

                                                                                                       September 2012 P E R S O N A L C A R E          5
ESSENTIAL OILS




Figure 6: A small plant designed and built by the author to                   Figure 7: A glassware still is usually more efficient than a
convert used cooking oil to bio-diesel.                                       commercial still.

fabrication and modification at a later date      to the US$200 per barrel mark, this is a              like palm oil wastes, but most of these
or restriction on the steam flow,                 critical issue for the existing industry and          remain pilot projects and may be too far
temperature and pressure that can be used         any potential new venture.                            away to consider.
in distillery operation. Some distillation            At the present, no specific alternative               Another alternative is solar distillation.
systems in remote areas of Australia and          sources of energy stand out as a solution.            Solar distillation involves using solar energy
Indonesia utilise a nearby pond to run a          Bio-diesel as an alternative to fossil fuels          to supply heat source to produce steam
pipe through where exiting vapours from           has gained a lot of attention at late, from           through a Scheffler mirror reflector to
the charge vessel are condensed and               either ethanol or a fixed oil feedstock, but          concentrate UV light onto a focal point to
collected on the other side of the pond,          pricing is still according to market forces,          convert water into steam.7 This method is
away from the distillery. This can be             usually around 70% to 90% of fossil fuels.            used to clean drinking water and is being
designed when one side of a pond is               The economics of jatropha cultivation and             used experimentally to distill essential oils.8
elevated from the other. Other ‘field’ or         extraction is questionable. The logistics of          The system does not work on cloudy days
‘bush’ stills utilise a large single water tank   producing your own is enormous due to                 where a backup system is required.
with stationary water inside to run a             the plant and land required and this type
condenser pipe through for the same               of venture would attract regulation,                  Required plant material throughput
effect. These methods save substantially          licensing and even excise in many legal               (Scale)
on the cost of constructing a dedicated           jurisdictions.6 However possibilities exist for       The required size of a distillery will depend
condenser.                                        the recycling of used cooking and engine              upon the required throughput of biomass
                                                  oils for diesel fuels. However in these               per annum and whether it will be a
Potential energy source                           cases collection and processing become                continuous or seasonal operation. The
One of the major challenges facing the            issues. Various pilot schemes exist in the            factors which should be considered in
essential oil industry today is final             region producing bio-fuels based on                   deciding upon the scale of the distillery
economical energy sources to produce              plastics, spent sugarcanes and other crops            would include:
steam. Stills in remote areas were directly
fired using firewood collected from
surrounding areas. However due to the                         Initial Parameters of                                Determination of distillation
decline in logging in most places, a                                Prototype                                      Time (according to various
                                                                    Still diameter                                        conditions)
premium has been put on the cost of fire
wood and for many places it is not free                              Still height
                                                                    Steam source
anymore. Plant refuse from the still can                             Steam type
be used for distillation, but it is only a                                                                         Determination of distillation
supplement to firewood, as there is not                                                                                   Stop point
enough volume in its own right to maintain
a distillery operation. Further there are                       Initial Distillation
alternative uses for plant refuse in                                Conditions
                                                                 Material preparation                                    Evaluate steam
mulching and composts which if applied                            Packing density                                  flow/temp/pressure to yield
correctly can save more on labour for                         Steam flow/temp/pressure
weeding and maintaining moisture in soils.                     Stop point of distillation
    Larger distilleries have employed diesel,
bunker fuel or natural gas to power their                                                                          Determination of steam flow/
                                                                                                                      Temp/pressure rates
boilers. With the crude oil price going                 Initial Distillation Results
above US$100 per barrel at the time of                             Oil Constituents
writing, up from just US$16 per barrel a                               Oil Yield
few years ago, the cost of running a                             Total oil verses time                            Further modification of
                                                                  Oil to water ratio                                       still
distillery in terms of fuel has risen fivefold.
Given that the market expects the price of
crude oil to rise even further, perhaps close     Figure 8: Testing procedure for prototype stills.

6     P E R S O N A L C A R E September 2012
ESSENTIAL OILS



ɀ Whether the harvest would be seasonal
  or staggered over the year.
ɀ The actual size of the plantation, i.e.,
  tonnage of bio-mass to be processed
  each year.
ɀ Whether labour is an important factor in
  the cost of production (operating cost),.
ɀ The value of the crop, and
ɀ The overall capital cost of the distillery.

If harvesting needs to be undertaken within
a short season, as would be the case for
peppermint, a large distillery to cope for
the biomass within the period would be
necessary. The number of operating hours
distillation is carried out in a day, i.e.,
single or double shift or around the clock       Figure 9: Manual harvesting and mulching before loading into fixed still arrangement
would also influence the required size.          at author’s property in Perlis, Malaysia.
Crops with less critical harvest times,
where harvesting can be staggered would              Fixed stills are ideal for operations that                  clamped during distillation. The foliage is
require a smaller distillery.                    require water distillation. They are also                       usually loaded and unloaded manually or
     The design of efficient working stills      suitable for plant material where heavy                         with the assistance of a block and tackle
usually comes with experimental trial and        comminution is required and this cannot                         pulley, connected to a tractor. Compact
error, and the testing of smaller prototype      be undertaken in the field. Most fixed stills                   packing of the charge into the still is vital
stills in field operation where they can be      exist in smaller to medium plantations and                      in achieving good yields. The charge must
scaled up. Field results will differ from        in operations where plant material is                           be packed efficiently to prevent steam from
laboratory results because; laboratory           collected from the wild. They are also used                     channelling through the plant material.
distillations will be exhaustive and field       in situations where the cost of labour is not                   Steam is usually generated through an
distillations will be guided by shut down        of paramount importance to the economics                        adjacent boiler, which can produce some
times. A laboratory distillation will utilise    of the operation, so many family farms in                       pressure. Steam is introduced into the
selected parts of the plant, where the field     Australia utilise this method as they are                       charge vessel through a pipe arrangement
distillation may also incorporate branches       owner operated. However, it should be                           or vapour coils to distribute the steam
and twigs because of the economics of            noted that due to rapidly rising living                         evenly. Others utilise a direct fire under the
harvesting them. Plant material in               standards in many parts of South East                           still, built up upon a three sided brick wall.
laboratory distillations will be packed          Asia, these operations could face                               A direct fire will only produce steam at
differently, milder steam will be used in        challenges to their economic viability.                         atmospheric pressure. Such stills usually
laboratory distillations and hydrophilic and         Most fixed stills consist of an open                        utilise water-steam distillation. Condensers
oxygenated compounds will be less in             topped tank, usually constructed of mild                        are either specially built or the natural
scaled up distillations.9                        steel or other locally available scrap                          topography around a pond or dam is used
     During the working life of each prototype   metals. The lid is usually sealed with cork                     as a cooling reservoir with the separator
still, a number of design parameters,            or mud, which is not heat sensitive and                         positioned on the other side of the dam.
operating procedures and plant
characteristics should be tried and tested
to determine their influence on results.                                 Lid with Clamps
                                                                                                                                            Corrugated Iron Condenser Tank
These are shown in Figure 8.                                                                                     Vapour Outlet Running
     Still scale varies from plantation to                                                                        into Corrugated Tank

plantation, with different ideas and
philosophies about the optimum size.
Some systems distil small batches at a                                     Distillation Vat
                                                                                                  Vapour Outlet Running Pipe for
                                                                                                                       “T”
time within a cartridge or bin system,             Counterweight                                   into Corrugated Tank Pressure
usually handling multiple units at a time.                                                                             Equalisation
Other systems distil a large charge at a
time. System design appears to be more
influenced by the logistic flow than the
technical issues of distillation. Most
                                                                                                                                      Oil
designs in larger scale operations are                                 Welded Steel Mesh Bottom
more concerned about continuous                                                                                                  Water
operational flows, minimising labour and
handling. No widespread conclusions have
been made about this issue. In plantations            Brick
                                                   Compartment          “Firebox” for wood fire
of medium size, one of three types of
systems are usually employed; a fixed
still operation which requires manual                                                                         Constant Level Separator
loading and unloading, a cartridge system                                                                         Tank
or a box system.                                 Figure 10: Simple design layout of a fixed still.

                                                                                                                 September 2012 P E R S O N A L C A R E                 7
ESSENTIAL OILS




Figure 11: A cartridge distillation system at the former ‘Maincamp’                 Figure 12: Box coupled to the steam source at the distillery for
property in Australia.                                                              peppermint distillation at Myrtleford, Victoria.

Alternatively a stationary tank is used to                   Box distillation systems are usually used inlet pipe is connected at the bottom of the
house cooling water for the condenser                   for extensive high biomass crops like mint                box and another pipe (or lid) connected at
pipe. Figure 10 shows a simple design                   and fennel, where a number of growers                     the top flowing to the condenser system.
diagram of a fixed still.                               over a particular area may share the                      Once the distillation has been completed,
    Cartridge distillation systems were                 facilities. A central distillery is made up of a the box is pulled out of the distillation
developed as a labour saving process over               steam boiler and a station to park and                    station and through hydraulics, tips out
fixed stills which have to be loaded and                connect up boxes to the steam and                         the spent plant material into a designated
unloaded manually. This system can exist                condenser. The box is mobile on a trailer                 refuse area, before being returned to the
in two basic forms. One is where plant                  that can be carted behind the harvester in                field.
material is brought in from the field and               the field for direct filling of                                Some producers use small compact
loaded into the cartridges at the distillery            the harvested plant material. The box will                boxes which are easier to use on fields,
and loaded into the still, once the previous            have a lid that can be elevated towards                   especially during rainy conditions. Smaller
cartridge has completed its distillation.               the harvester, so the harvested material                  boxes can be distilled quicker and are
The other is where the cartridge is actually            can be deposited or with no lid, where a                  lighter in weight for handling and most
taken into the field behind the harvester               suspended lid at the distillery will be                   suitable when the distillery is nearby.
and loaded directly during the harvest.                 lowered onto the box during the actual                    Smaller boxes also create less pressure at
    These systems greatly improve the                   distillation. Once the box is full of plant               the beginning of a distillation when the
logistics of distillation, where cartridges             material, it is disconnected from the                     massive air volume in the top of box heats
can be positioned ready for exchange with               harvester and attached to a truck or tractor up and is expelled through the condenser
the previously distilled cartridge, almost              (depending on the distance) for transport                 system. Larger boxes, although more
immediately without having to wait for the              to the distillery. At the distillery, a steam             difficult to handle on the field, lend
spent plant material to cool.                                                                                                      themselves to longer distance
Distilled cartridges are lifted to                                                                                                 hauls to a central distillery.
a refuse area where the spent                                                                                                           The box must be designed so
foliage is tipped into a compost                                                               Each box can be distilled on rotation
                                                                                                                                   that steam will circulate
                                                                                               or both together, governed by boiler
heap, before the cartridge is                                                                               capacity.              throughout the space inside the
returned to the field. In some                                                                                                     box. Design of the internal
systems, the cartridges                                                        Boiler
                                                                                                                                   piping array to inlet the steam is
themselves                                                                                                                         critical. The herb material rests
form the still, where the steam                                                                                                    on a false mess bottom above
inlet pipe and vapour outlet                                                                                                       the steam inlets to prevent any
are connected directly to the                                                                                                      burning of foliage that could
steam boiler and condenser                                                                                                         create unpleasant odours and
respectively, for immediate                                                                                                        assist in even distribution of the
distillation.                                                                                                                      steam vapour throughout the
    These designs greatly                                                                                                          internal space of the box. Box
improve daily production                                                                                                           stills are suitable for logistic
throughput, as loading, cooling                                                                                                    situations where crops are
and unloading times between                                                                                                        grown in distributed areas, as
                                                 Box No. 1.                                           Box No. 2.
distillations are saved. Still                                                                                                     transport of herb material is a
heights range between 1.3-2.0                                                                                                      crucial issue. Box systems are
                                                                                                    Condensers
metres with a suitable diameter                                                                                                    also very efficient from the
for handling. Still design is                                                                                                      labour point of view, requiring
                                        Boxes driven in by tractor
greatly influenced by handling          and coupled up to steam                                                                    only one person to drive the
convenience. The steam supply             inlet and condenser.                                                                     harvester, one person to drive
should be sufficient to handle                                                                      Separators                     the transporter, one person to
multiple charges at one time                                                                                                       operate the steam and one
for best efficiency.                   Figure 13: Layout plan for a box system distillery.                                         person to couple and uncouple

8      P E R S O N A L C A R E September 2012
ESSENTIAL OILS


the boxes and pipes during the operation.        mulch as it has been sterilised during                  flowers: live or dead – which do we want? In:
                                                 distillation. The farm enterprise has the               Lawrence BM, Mookherjee BD, Trenkle RW eds.
Distillation effluent                            option of either using the mulch back on                Flavors and fragrances: a world perspective.
A distillation plant will have two types of      its own fields or selling it as a commercial            Proceedings of the 10th International Congress
polluting effluent, smoke from a steam           product. There is usually high demand for               of Essential Oils, Fragrances and Flavors,
generator (unless electrically powdered)         good mulches in the horticulture,                       Washington DC. Amsterdam: Elsevier Science
and the water distillate from the charge         agriculture and home gardening sectors.                 Publishers, 1986: 415-24.
bin. These effluents fall under the                   Other potential by-products from               5   Mookherjee BD, Trenkle RW, Wilson RA. Live vs.
jurisdiction of local environmental              distillation wastes include hydrosols from              dead (Part II): a comparative analysis of the
protection authorities. Smoke discharges         certain distillate waters, although these are           headspace volatiles of some important
may require filters to trap excess carbon        limited to a few crops like lavender, rose,             fragrance and flavor raw materials. Journal of
emissions and distillation effluent may          and other florals. Spent foliage can be                 Essential Oil Research 1989; 2: 85-90.
require aerobic or anaerobic treatment in        used as cattle feed base, ferro-cement              6   Menage E, Nicholson K. Used oil as an
a pond before discharge into the                 filler for green bricks and buildings, and as           alternative boiler fuel- promises and problems,
environment.                                     a source of fuel for steam production in                Southeastern apos; 93, Proceedings, Charlotte,
                                                 the distillation plant.                    PC           NC. IEEE, 4-7 April, 1993.
Potential by-products from                                                                           7   For layouts and plans see: Dupont F. Essential
the distillation process                         References                                              oil extraction from herbs using solar energy – a
The production of any possible by-               1 Clark RJ, Read C. Production of peppermint oil:       thesis summary. http://www.uni-kassel.de/fb11/
products from the waste products of                a model of best practice for Tasmania and             agrartechnik/Fachgebiet/personal/Florent/
distillation, not only assists in the handling     Victoria, Canberra. A report for the Rural            Florent_Thesis_summary.pdf (accessed 7th
of wastes, but in adding value to the              Industries Research and Development                   January 2009).
process through either savings or extra            Corporation, August 2000, p61.                    8   Munir A, Hensel O. Development of a solar
revenue gained.                                  2 Hunter M. Essential oils: art, agriculture,           distillation system for essential oils extraction
    The spent foliage of many plants after         science, industry and entrepreneurship: a focus       for herbs – Conference on Utilisation of diversity
distillation can by utilised as mulch. Mulch       on the Asia-Pacific Region. New York: Nova            in land use systems: Sustainable and organic
is very beneficial in weed control and             Scientific Publishers, 2009: p417                     approaches to meet human needs. Tropentag,
maintaining moisture in the soil after rain      3 Matile P Altenburger R. Rhythms of fragrance
                                                            ,                                            9-11 October 2007. http://www.tropentag.de/
or irrigation. Using spent foliage as mulch        emission in flowers. Planta 1988: 174:                2007/abstracts/links/Hensel_4GdqiE2W.pdf
is also part of a sustainable farming              242-7.                                                (accessed 7 January 2009).
system and encouraged. Spent foliage             4 Mookherjee BD, Trenkle RW, Wilson RA,             9   Mateus EM, Lopes C, Nogueira T, Lourenco
after oil extraction usually makes good            Zampino M, Sanads KP Mussinan CJ. Fruits and
                                                                           ,                             JAA, Curto MMJ. Pilot steam distillation of




                                                                                                     September 2012 P E R S O N A L C A R E               9

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The Distillation of Essential Oils Part 3

  • 1. Murray Hunter – University Malaysia Perlis ESSENTIAL OILS The distillation of essential oils 3: PART The final part of this series on distillation carries on from the basic principles, stages and types of distillation to look at harvesting, selection and design of a distillation system, and the scaling up process. Harvesting However under plantation The method and timing of cultivation, the whole tree is harvesting crops will depend coppiced at an early stage, upon the part of the plant where it will usually re-grow required, the pre-processing increasing leaf biomass for preparation required before future harvests. This is also the extraction, the re-growth case with tea tree (Melaleuca characteristics of the crop, alternifolia) where initial growth the changes of chemical from a seedling will have a constituents in the plant during singular trunk where coppicing growth, the diurnal variance of after the first year and breaking chemical constituents in the up the trunk butt at ground plant, the characteristics of the level, will promote multiple field and the type of enterprise stem re-growth, promoting in terms of size, scale and more biomass (Fig. 1). Table 1 socio-economic environment shows the length of the first it operates within. Figure 1: Broken up tea tree trunk to promote coppice growth. harvest time from planting As essential oils can be and method of harvest. sourced from leaves, stems, flowers, bark, combing them from branches in some Some crops like peppermint have a wood, fruits, rhizomes or seeds, the nature instances. distinct harvest window where phyto- of the plant material required will have With trees like eucalyptus and lemon chemicals within the leaves synthesise and great bearing on the mode of harvesting myrtle, a portion of the leaves are usually convert into desirable constituents that required. lopped off for distillation, leaving the bulk give the oil its commercial value. These Flowers are more delicate than other of the tree intact for growth. These trees, processes depend upon seasonal factors plant tissues and mechanisation may if mature in the wild, will have difficulty and temperature conditions, i.e., in the damage them. Thus many flowers like re-growing if completely chopped down. case of peppermint daylight hours and rose and cananga must be picked manually. Some jasmine and boronia are mechanically harvested through combing Optimum harvest window 80 80 arrays, although the effectiveness of this is unknown. Bark can be scraped off from 70 70 trees or collected as a by-product of the timber industry. However many bark 60 Oil yield 60 products come from remote areas in Yield (kg/ha tropical countries and are still collected 50 50 % in oil manually by collectors from both the wild and plantations. Woods have to be cut in a 40 40 Menthol similar manner to how the timber industry 30 30 would harvest a tree. Fruits are usually utilised for other products like citrus juices, Menthone 20 20 and the peels which contain oil are processed as a by-product. Rhizomes must 10 Methyl acetate 10 be collected from underground, either Menthofuran manually or through mechanical upturning 1 2 3 4 5 6 7 8 9 10 11 12 of the earth. Seeds are either directly Weeks from 1 January collected from the ground or plant when mature via manual or mechanically Figure 2: The harvest window applicable to the Victorian and Tasmanian mint industries. September 2012 P E R S O N A L C A R E 1
  • 2. ESSENTIAL OILS night time temperatures. Plants like Artemisia vulgaris change in constituent levels throughout their growth cycle, so it is important to determine the optimal harvest time based on maturity.1 Determining the optimal harvest time requires sampling and graphing of the leaf oil constituents over the crop lifecycle. Figure 2 shows the harvest window applicable to the Victorian and Tasmania mint industry in Australia.2 Some flowers exhibit diurnal variations in constituents and the daily timing of harvest is critical. This is the case for rose and jasmine which may have to be harvested in the very early hours of the morning to obtain the optimum constituents in the flowers for extraction. Other flowers where this issue is important include Hoya carnosa, Stephanotis floribunda,3 Syringa vulgaris,4 Narcissus tazetta and Osmanthus fragrans.5 Harvesting methods and timing are Figure 3: Paddle arrangement connected to tractor wheel for ‘boggy’ conditions Table 1: The length of harvest time and method of harvest for some essential oil crops. Common name Time from initial planting to first harvest Method of harvesting Australian Tea Tree Usually can make first harvest 8-12 months Usually mechanised harvesting where the whole tree is cut and Melaleuca alternifolia after planting. Second and subsequent mulched for easy distillation. First harvest tree will be a single trunk, harvest every 6-13 months, depending but after harvest stump is smashed so tree can coppice many trunks. upon climate. Manual harvest is undertaken in Malaysia, Cambodia, etc. Basil, Ocimum basilicum Plants usually flower at 50-60 cm height Plants are cut immediately upon flowering, either manually or and sub-species. after 3-6 months. mechanically. Basil should be replanted after harvest. Black Pepper, Harvested when plants fruit, just when they start to ripen. Piper nigrum This is usually a manual operation and occurs several times during the season. Calamus Oil, Usually can be harvested 6-10 months after Rhizomes must be dug up by spade or plough, washed and dried before Acorus calamus planting distillation. Cananga/Ylang Ylang Usually in 2nd year, peak after 5th year. Manual picking: Flowers should be picked when early in the morning to Cananga odoratum maximise oil content, only after they have turned yellow. Ropes are sometimes attached to the branches so pickers can pull them down to pick off the flowers without having to climb the tree. Cassia Bark, various Cinnamomum cassia: First harvest approximately Cinnamomum cassia: Trees coppiced and pruned by hand to strip leaves Cinnamomum species 5-7 years when trees coppiced at 3 m height. and bark for oil production. Cinnamomum verum: first harvest 2-3 years Cinnamomum verum: Tree coppiced at 3 m height after 2 years for after planting bark by hand. Citronella, Cymbopogon Usually first harvest can be undertaken between Small holders will manually harvest with a sickle and carry to the nardus 4-5 months after initial planting, with still for distillation. Foliage harvesters are used on larger fields, which subsequent harvests every 3-4 months. chop and collect the material. Most oil is in the leaves so cutting distance set to where the bulk of the leaves are (18-28 cm). This also allows faster regrowth. Crop can have a commercial life of 4-10 years. Coriander seed, Usually after 6 months with coordinated spring When the plant is 50-70 cm in height and fruit is 5-7 mm in size Coriandrum sativum planting and autumn harvest. Geranium, many species Crop usually grows enough foliage for first Usually mowed around 10-15 cm above the ground as little oil in the and hybrids of harvesting 6-9 months after planting stems [143] and to allow for re-growth. Pelargonium Ginger, Zingiber officinale Harvest can occur anywhere between 150-300 It is important to determine the optimal level of oil and oleoresin content and other species days after planting, depending upon temperature in the rhizomes before harvesting. Harvesting can be manual or conditions. mechanised, as whole plant is pulled out, which must be without damage. Jasmine, various Jasmine may take 4-5 years before productive. In warm humid areas, flowers can be continually harvested for around Jasminum species. 6-9 months per year. Flowers should be picked before sun rises 20% above the horizon and a daily basis to avoid loss of volatiles. This is a manually process, although combing and suction systems have been experimented with. Plants are usually pruned after each flowering season to promote growth. 2 P E R S O N A L C A R E September 2012
  • 3. ESSENTIAL OILS affected by the physical state of the as is in the case of patchouli where it must the tyres of the harvesting equipment, so fields. Hilly fields restrict the degree of be stored before distillation. that the crop can be effectively harvested. mechanisation during harvesting, An important consideration in the design Planning of the harvest is of paramount particularly if the gradients are high. of any harvesting system is the potential importance as it must be synchronised with The weather, particularly rain, will degrade damage on the plant material. Some plant the capacity of the distillery to ensure there field compactness and can lead to delays material is very easily bruised or damaged, is no undesired backlog of unprocessed in harvesting as conventional harvest which would restrict mechanisation options. material waiting to be distilled. Ideally, equipment may have trouble operating on This is why some traditional harvesting harvest should be followed by almost waterlogged fields, particularly in tropical methods are still widely used for a number immediate distillation, where appropriate. areas. Mechanised harvesting equipment of essential oil crops. The distance of the field from the distillery can be adapted to waterlogged fields The most efficient method of harvesting is also a consideration and harvest times through paddle arrangements connected is to cut the material in the field and load over a diverse region utilising a central to the wheels of tractors and bins. it directly into a container that will also act facility, requires very careful logistical This method is successfully used in rice as the charge vessel during distillation. This planning. Where crops like mint require paddies throughout South-East Asia. causes some loss of oil and inefficiency in some time to wilt after being mowed before The harvesting system should ideally yields due to non oil-bearing plant material being picked up by a forage harvester and be integrated with the extraction system also being harvested, i.e., twigs and deposited into buns, delays in the two for maximum efficiency. This is restricted branches in tree crops. But overall this operations can lead to excessive wilting, by any pre-extraction wilting and/or is much more economic than selective which will greatly reduce oil yields. Wilting comminution required before extraction, harvesting of plant parts. If crops are times may be heavily influenced by daily as any pre-processes increase the time mechanically harvested, row planting must wind and temperature conditions, requiring lag between harvest and extraction, such be coordinated with the distance between great flexibility in the time lag between Table 1 (continued): The length of harvest time and method of harvest for some essential oil crops. Common name Time from initial planting to first harvest Method of harvesting Lemon scented gum, First harvest 6-12 months after planting. If grown solely for oil production, trees should be regularly topped and Eucalyptus citriodora After 2nd year tree can be felled for re-growth. coppiced to maintain growth. A height of around 2.5 m maintained. Alternatively trees can be felled, leaving the main stem for re-growth of a coppice of young shoots, which can be re-harvested every 6-12 months. Lemon Scented Tea First harvest after 2-3 years, subsequent A foliage harvester can coppice the tree when re-growth warrants it. Tree, Leptospermum harvests each year. petersonii Lemongrass, Usually first harvest can be undertaken between Small holders will manually harvest with a sickle and carry to the still for Cymbopogon flexuosus 4-7 months after initial planting with subsequent distillation. Foliage harvesters are used on larger fields, which chop and harvests every 3-5 months. collect the material. Most oil is in the leaves so cutting distance set to where the bulk of the leaves are (15-20 cm). This also allows faster regrowth. Crop can have a commercial life of 4-5 years. Nutmeg, Myristica Trees from seed bear fruit between 6-10 years, Fruit is allowed to split and either picked or allowed to fall to the ground fragrans vegetative propagated trees 5-7 years. and collected on a daily basis. Nets can also be used to catch the Fruit ripens around 6-9 months after flowering. falling fruits. Long poles with cutters also used. Reach maximum yields after 20 years. Palmarosa, Cymbopogon First harvest around 6 months after planting Plants should be mechanically or manually harvested about 10 cm from martini var. motia Further harvests when flowering occurs every the ground, when flowering begins, around 6 months after planting. and sofia. 6 months. Patchouli, Pogostemon Can be harvested 4-8 months after planting Usually the leaves are cut manually or mechanically, dried and stored to cablin and subsequent harvests at 3-6 month allow some fermentation, before distillation at a later time. intervals for a 2 to 6 year period. Peppermint, Mentha Planted in early spring and harvested mid to The crop is usually mowed, allowed to wilt and them scooped up into piperita late summer. bins for distillation. This is usually an automated process. Rose, Rosa species Flowers picked manually between 5-10 am in the morning, (usually R. centifolia while flowers still open. and damascena) Sage, Salvia officinalis Trees can be trimmed after first year for Trees can be trimmed for leaves each year and dried. around 6 years. Sandalwood, Santalum 30-50 years after planting The oil is contained primarily in the heartwood and large roots, thus the album and S. spicatum tree must be felled and pulverized. Tasmanian Blue Gum, Trees can be lopped after 6-12 months, upon Trees either coppiced and lopped when dedicated to oil production Eucalyptus globulus reaching around 3 m height. Trees then allowed manually or through mechanized lopper. If trees cultivated for timber, to coppice for lopping and coppicing every harvest after tree felled around 5-8 years of age. 9-15 months. Vertivert, Vetiveria First harvest usually 18 months after planting to Usually the foliage is cut and slashed prior to the lifting of rhizomes zizanioides allow rhizomes time to mature. (sometimes burning used). Roots either dug up manually or dug up with the aid of a mechanical digger. As much vetiver is planted on hill slopes, harvesting is a very difficult process to mechanise. September 2012 P E R S O N A L C A R E 3
  • 4. ESSENTIAL OILS mowing and picking up the foliage for ɀ Efficient collection of the material in the these systems will fulfill their requirements. distillation. field and delivery to the distillery. Fabricated ‘turnkey systems’ are offered by Still today a large amount of harvesting ɀ Minimisation of backlogs in material to some suppliers, however, they account only is undertaken either manually as is the be distilled, and for a small percentage of actual working case in Indonesia, Cambodia and Vietnam ɀ Minimal delays in harvest to distillation field stills in the industry. Most stills are by small holders. ‘Outback’ stills are still times, according to requirements. locally fabricated with local materials taking used in Australia for tea tree, where the advantage of the local topography and farmer collects wild or small scale Selection and design energy sources, usually fitting in with the plantation material with a tractor and of extraction system socio-cultural way cultivation is undertaken trailer, to be loaded into the still upon The choice of method for essential oil in their geographical location. This would returning from the field. Although some extraction will depend upon: include the majority of small holder companies offer state of the art harvesting ɀ The sensitivity of the aromatic production, cultivating small plots or equipment, many producers fabricate their constituents in the plant to heat. collecting from the wild in Indonesia and own specialised equipment, utilising ɀ The sensitivity of the aromatic Vietnam. Similarly, boutique farms standard agricultural machinery available. constituents in the plant to moisture. producing specialty essential oils like Over a period of years during the winter ɀ The volatility of various constituents lavender, tea tree, manuka and lemon months, this equipment is rebuilt and within the plant. myrtle in Australia and New Zealand would modified to suit their small to medium ɀ The physical nature of the plant tissue. also in the majority of cases employ simple scale operations. Large scale operations in ɀ The solubility in water of the aromatic designs. Only large extensive farms the mint, citrus, eucalyptus and tea tree constituents within the plant. producing large tonnage oil like mint and industries utilise equipment that brings the the larger Australian tea tree plantations most efficiency to the operation, as a low An overview of some of the issues involved would develop capital intensive ‘integrated production cost is of great importance to in selecting an extraction process can be production systems’. survival. seen in Figure 4. A number of factors must be taken into Good management of the harvesting A summary of the extraction methods consideration when designing a distillation procedure requires: used for a number of essential oils is listed system for the project: ɀ The determination of the optimal harvest in Table 2. time. The comments in the rest of this The nature of the plant material ɀ Precise mowing or harvesting of the section are primarily related to distillation. This would lead to considerations such as; herb with minimal damage to the crop. A great number of distilleries tend to be what are the absorption characteristics of ɀ Consistent and precise wilting, if locally built and designed from what the material? What would the most required before extraction. information people have in the hope that important distillation fundamentals that Table 2: Methods of extraction utilised for a number of essential oils. Essential oil Botanical name Part of plant used for extraction Usual method(s) of extraction Star anise oil Illicium verum Seeds Steam distillation after seeds are comminuted Artemisia oil Artemisia vulgaris All the herb Steam distilled after drying Basil oil Ocimum basilicum All the herb Steam distilled after drying Bergamot oil Citrus bergamia Fruit Peels Cold expression of nearly ripe fruits Broom absolute Spartium junceum Flower blossoms Solvent extraction Cajuput oil Various Melaleuca species Leaves and twigs Steam distillation of fresh material Calamus oil Acorus calamus Roots Steam distillation of fresh or dried material Cananga oil Cananga odorata Flowers Steam distillation of fresh material Cedarwood oil Juniperus virginiana Wood chips, sawdust Steam distillation Celery Seed oil Apium graveolens Seeds Steam distillation of crushed seeds Citronella oil Cymbopogon nardus Grass Steam distillation of dried material Coriander seed oil Coriandrum sativum Seeds Steam distillation fo crushed dried seeds Fennel oil Foeniculum vulgarie Seeds (in fruits) Steam distillation of the crushed seeds Ginger oil Zingiber officinale Rhizomes Steam distillation of freshly ground rhizomes Jasmine absolute Jasminum grandifloram and other Flowers Solvent extraction of the fresh flowers Lavender oil Lavandula officinalis and others Flowering tops and stalks Steam distillation of fresh material Lemon oil Citrus medica Peel Cold expression Lemongrass oil Cymbopogon flexuous and citratus Grass Steam distillation of fresh or mildly wilted grass Lime oil Citrus aurantifolia Peels Steam distilled or cold pressing Litsea Cubeba oil Litsea cubeba tree Ripe fruit Steam distillation Patchouli oil Pogostemon cablin Leaves Steam distillation of dried and fermented leaves under pressure Rose oil Rosa centifolia, damascena and others Flowers Water distillation of fresh flowers Sandalwood oil Santalum album Wood Steam distillation of chipped and powdered wood Thyme oil Thymus vulgaris Flowering herb Steam distillation 4 P E R S O N A L C A R E September 2012
  • 5. ESSENTIAL OILS would apply to this material? What would be the effect of steam and/or water on the physical state of the material (i.e., will it congeal or tend to form steam channels)? Will the material have to be pre-processed before distillation (i.e., cut up, ground or Influencing Factors Historical some other form of comminution)?. Is the Compound characteristics material sensitive to delay in distillation? (volatility/mol. Weight) Does it have to be wilted? Are the volatile Surrounding Material Compounds Highly volatile mixed with terpenes constituents subject to damage at waxes, also prolonged high temperatures? Are there lactones, Low/medium volatility/stable esters etc. low and high boiling constituents? What considerations must be given to this? Distillation Solvent Cold How do others distill this material? Extraction Pressing These questions would assist in identifying the most suitable type of Automated distillation method and the general harvest and practices that will be applied during Influencing Factors Harvest and distillation Price vis. Market later load system system distillation, such as what type of steam, Volume for how long should it be distilled, etc. Plant cell structures Field size Topography The harvest method and logistics Soil/field characteristics The harvest methods used will depend Part of plant (i.e., Extensive rhizome/leaf) Manual large scale upon the scale of the project, the nature of Coppice High --- Low harvesting farming the herb, the local traditions and practices Value due to of farming, the capital investment made scale, into the venture and the amount of the material, Specialties Distillation investment particular herb that requires handling and processing. Harvest methods can vary from manual harvesting, mowing and wilting Hydro Material before being picked up from the field by Characteristics ‘Finer’ another vehicle, to a fully integrated system CO2 composition spectrum where the material is harvesting, mulched Solubility in Water-Steam and spread directly into a cartridge or box water Individual array, behind the tractor/harvester. Another Fractional aroma Distillation consideration is the potential damage that compounds could occur to the plant material through Steam Material Characteristics harvesting, as in the example of rose petals which must be picked by hand to prevent A Basic Harvest to Distillation Flowchart for any damage which could promote Peppermint Oil Figure 4: Some of the factors influencing the mode of extraction of essential oils from plants. hydrolysis, oxidation and resinisation before distillation. Time between harvest and distillation is another factor that needs Determination of Harvest time (Sampling) consideration. In the case of rose petals, distillation time after harvest is very crucial, where time is not as critical for eucalyptus 10 tonne fresh herb per Ha. Mowing and leaving to wilt on and tea tree oil distillation. Basically a field Fresh herb contains 80% ‘time and motion’ flowchart of the logistical moisture aspect of harvest to distillation can be undertaken, which can assist in Wilting Must wilt to 50% moisture determining the amount of integration level where ‘crisp and brittle’ between harvesting and distillation systems. This needs to be quantified with Pick up with forage harvester expected volumes on a daily basis to assist Collect 6 tonne of dry herb in determining the required still capacity, steam requirements and overall still design. Must insure that herb is not A flowchart for mint is shown in Figure 5. Deliver to Distillation system bruised. Use cartridge or box to avoid too much handling Available cooling water for condenser Volume of 4 M2 per tonne An important factor in condenser design is of herb. Distillation the temperature of the available water If single charge, yield 15kg oil for cooling. This will greatly influence the Assume 35 minutes distillation time, 10 size of the condenser along with vapour minutes change over, 6.90 litres/minute If distillate ratio is 0.062/1 steam rate per minute. 9 hours will handle (oil/water), then 241.8 litres throughput. Ignoring the condensate water 12 tonnes of dried herb in a vat of 4m 3. water required for distillation. temperature issue when designing the condenser could lead to expensive re- Figure 5: A basic harvest to distillation flowchart for peppermint oil. September 2012 P E R S O N A L C A R E 5
  • 6. ESSENTIAL OILS Figure 6: A small plant designed and built by the author to Figure 7: A glassware still is usually more efficient than a convert used cooking oil to bio-diesel. commercial still. fabrication and modification at a later date to the US$200 per barrel mark, this is a like palm oil wastes, but most of these or restriction on the steam flow, critical issue for the existing industry and remain pilot projects and may be too far temperature and pressure that can be used any potential new venture. away to consider. in distillery operation. Some distillation At the present, no specific alternative Another alternative is solar distillation. systems in remote areas of Australia and sources of energy stand out as a solution. Solar distillation involves using solar energy Indonesia utilise a nearby pond to run a Bio-diesel as an alternative to fossil fuels to supply heat source to produce steam pipe through where exiting vapours from has gained a lot of attention at late, from through a Scheffler mirror reflector to the charge vessel are condensed and either ethanol or a fixed oil feedstock, but concentrate UV light onto a focal point to collected on the other side of the pond, pricing is still according to market forces, convert water into steam.7 This method is away from the distillery. This can be usually around 70% to 90% of fossil fuels. used to clean drinking water and is being designed when one side of a pond is The economics of jatropha cultivation and used experimentally to distill essential oils.8 elevated from the other. Other ‘field’ or extraction is questionable. The logistics of The system does not work on cloudy days ‘bush’ stills utilise a large single water tank producing your own is enormous due to where a backup system is required. with stationary water inside to run a the plant and land required and this type condenser pipe through for the same of venture would attract regulation, Required plant material throughput effect. These methods save substantially licensing and even excise in many legal (Scale) on the cost of constructing a dedicated jurisdictions.6 However possibilities exist for The required size of a distillery will depend condenser. the recycling of used cooking and engine upon the required throughput of biomass oils for diesel fuels. However in these per annum and whether it will be a Potential energy source cases collection and processing become continuous or seasonal operation. The One of the major challenges facing the issues. Various pilot schemes exist in the factors which should be considered in essential oil industry today is final region producing bio-fuels based on deciding upon the scale of the distillery economical energy sources to produce plastics, spent sugarcanes and other crops would include: steam. Stills in remote areas were directly fired using firewood collected from surrounding areas. However due to the Initial Parameters of Determination of distillation decline in logging in most places, a Prototype Time (according to various Still diameter conditions) premium has been put on the cost of fire wood and for many places it is not free Still height Steam source anymore. Plant refuse from the still can Steam type be used for distillation, but it is only a Determination of distillation supplement to firewood, as there is not Stop point enough volume in its own right to maintain a distillery operation. Further there are Initial Distillation alternative uses for plant refuse in Conditions Material preparation Evaluate steam mulching and composts which if applied Packing density flow/temp/pressure to yield correctly can save more on labour for Steam flow/temp/pressure weeding and maintaining moisture in soils. Stop point of distillation Larger distilleries have employed diesel, bunker fuel or natural gas to power their Determination of steam flow/ Temp/pressure rates boilers. With the crude oil price going Initial Distillation Results above US$100 per barrel at the time of Oil Constituents writing, up from just US$16 per barrel a Oil Yield few years ago, the cost of running a Total oil verses time Further modification of Oil to water ratio still distillery in terms of fuel has risen fivefold. Given that the market expects the price of crude oil to rise even further, perhaps close Figure 8: Testing procedure for prototype stills. 6 P E R S O N A L C A R E September 2012
  • 7. ESSENTIAL OILS ɀ Whether the harvest would be seasonal or staggered over the year. ɀ The actual size of the plantation, i.e., tonnage of bio-mass to be processed each year. ɀ Whether labour is an important factor in the cost of production (operating cost),. ɀ The value of the crop, and ɀ The overall capital cost of the distillery. If harvesting needs to be undertaken within a short season, as would be the case for peppermint, a large distillery to cope for the biomass within the period would be necessary. The number of operating hours distillation is carried out in a day, i.e., single or double shift or around the clock Figure 9: Manual harvesting and mulching before loading into fixed still arrangement would also influence the required size. at author’s property in Perlis, Malaysia. Crops with less critical harvest times, where harvesting can be staggered would Fixed stills are ideal for operations that clamped during distillation. The foliage is require a smaller distillery. require water distillation. They are also usually loaded and unloaded manually or The design of efficient working stills suitable for plant material where heavy with the assistance of a block and tackle usually comes with experimental trial and comminution is required and this cannot pulley, connected to a tractor. Compact error, and the testing of smaller prototype be undertaken in the field. Most fixed stills packing of the charge into the still is vital stills in field operation where they can be exist in smaller to medium plantations and in achieving good yields. The charge must scaled up. Field results will differ from in operations where plant material is be packed efficiently to prevent steam from laboratory results because; laboratory collected from the wild. They are also used channelling through the plant material. distillations will be exhaustive and field in situations where the cost of labour is not Steam is usually generated through an distillations will be guided by shut down of paramount importance to the economics adjacent boiler, which can produce some times. A laboratory distillation will utilise of the operation, so many family farms in pressure. Steam is introduced into the selected parts of the plant, where the field Australia utilise this method as they are charge vessel through a pipe arrangement distillation may also incorporate branches owner operated. However, it should be or vapour coils to distribute the steam and twigs because of the economics of noted that due to rapidly rising living evenly. Others utilise a direct fire under the harvesting them. Plant material in standards in many parts of South East still, built up upon a three sided brick wall. laboratory distillations will be packed Asia, these operations could face A direct fire will only produce steam at differently, milder steam will be used in challenges to their economic viability. atmospheric pressure. Such stills usually laboratory distillations and hydrophilic and Most fixed stills consist of an open utilise water-steam distillation. Condensers oxygenated compounds will be less in topped tank, usually constructed of mild are either specially built or the natural scaled up distillations.9 steel or other locally available scrap topography around a pond or dam is used During the working life of each prototype metals. The lid is usually sealed with cork as a cooling reservoir with the separator still, a number of design parameters, or mud, which is not heat sensitive and positioned on the other side of the dam. operating procedures and plant characteristics should be tried and tested to determine their influence on results. Lid with Clamps Corrugated Iron Condenser Tank These are shown in Figure 8. Vapour Outlet Running Still scale varies from plantation to into Corrugated Tank plantation, with different ideas and philosophies about the optimum size. Some systems distil small batches at a Distillation Vat Vapour Outlet Running Pipe for “T” time within a cartridge or bin system, Counterweight into Corrugated Tank Pressure usually handling multiple units at a time. Equalisation Other systems distil a large charge at a time. System design appears to be more influenced by the logistic flow than the technical issues of distillation. Most Oil designs in larger scale operations are Welded Steel Mesh Bottom more concerned about continuous Water operational flows, minimising labour and handling. No widespread conclusions have been made about this issue. In plantations Brick Compartment “Firebox” for wood fire of medium size, one of three types of systems are usually employed; a fixed still operation which requires manual Constant Level Separator loading and unloading, a cartridge system Tank or a box system. Figure 10: Simple design layout of a fixed still. September 2012 P E R S O N A L C A R E 7
  • 8. ESSENTIAL OILS Figure 11: A cartridge distillation system at the former ‘Maincamp’ Figure 12: Box coupled to the steam source at the distillery for property in Australia. peppermint distillation at Myrtleford, Victoria. Alternatively a stationary tank is used to Box distillation systems are usually used inlet pipe is connected at the bottom of the house cooling water for the condenser for extensive high biomass crops like mint box and another pipe (or lid) connected at pipe. Figure 10 shows a simple design and fennel, where a number of growers the top flowing to the condenser system. diagram of a fixed still. over a particular area may share the Once the distillation has been completed, Cartridge distillation systems were facilities. A central distillery is made up of a the box is pulled out of the distillation developed as a labour saving process over steam boiler and a station to park and station and through hydraulics, tips out fixed stills which have to be loaded and connect up boxes to the steam and the spent plant material into a designated unloaded manually. This system can exist condenser. The box is mobile on a trailer refuse area, before being returned to the in two basic forms. One is where plant that can be carted behind the harvester in field. material is brought in from the field and the field for direct filling of Some producers use small compact loaded into the cartridges at the distillery the harvested plant material. The box will boxes which are easier to use on fields, and loaded into the still, once the previous have a lid that can be elevated towards especially during rainy conditions. Smaller cartridge has completed its distillation. the harvester, so the harvested material boxes can be distilled quicker and are The other is where the cartridge is actually can be deposited or with no lid, where a lighter in weight for handling and most taken into the field behind the harvester suspended lid at the distillery will be suitable when the distillery is nearby. and loaded directly during the harvest. lowered onto the box during the actual Smaller boxes also create less pressure at These systems greatly improve the distillation. Once the box is full of plant the beginning of a distillation when the logistics of distillation, where cartridges material, it is disconnected from the massive air volume in the top of box heats can be positioned ready for exchange with harvester and attached to a truck or tractor up and is expelled through the condenser the previously distilled cartridge, almost (depending on the distance) for transport system. Larger boxes, although more immediately without having to wait for the to the distillery. At the distillery, a steam difficult to handle on the field, lend spent plant material to cool. themselves to longer distance Distilled cartridges are lifted to hauls to a central distillery. a refuse area where the spent The box must be designed so foliage is tipped into a compost Each box can be distilled on rotation that steam will circulate or both together, governed by boiler heap, before the cartridge is capacity. throughout the space inside the returned to the field. In some box. Design of the internal systems, the cartridges Boiler piping array to inlet the steam is themselves critical. The herb material rests form the still, where the steam on a false mess bottom above inlet pipe and vapour outlet the steam inlets to prevent any are connected directly to the burning of foliage that could steam boiler and condenser create unpleasant odours and respectively, for immediate assist in even distribution of the distillation. steam vapour throughout the These designs greatly internal space of the box. Box improve daily production stills are suitable for logistic throughput, as loading, cooling situations where crops are and unloading times between grown in distributed areas, as Box No. 1. Box No. 2. distillations are saved. Still transport of herb material is a heights range between 1.3-2.0 crucial issue. Box systems are Condensers metres with a suitable diameter also very efficient from the for handling. Still design is labour point of view, requiring Boxes driven in by tractor greatly influenced by handling and coupled up to steam only one person to drive the convenience. The steam supply inlet and condenser. harvester, one person to drive should be sufficient to handle Separators the transporter, one person to multiple charges at one time operate the steam and one for best efficiency. Figure 13: Layout plan for a box system distillery. person to couple and uncouple 8 P E R S O N A L C A R E September 2012
  • 9. ESSENTIAL OILS the boxes and pipes during the operation. mulch as it has been sterilised during flowers: live or dead – which do we want? In: distillation. The farm enterprise has the Lawrence BM, Mookherjee BD, Trenkle RW eds. Distillation effluent option of either using the mulch back on Flavors and fragrances: a world perspective. A distillation plant will have two types of its own fields or selling it as a commercial Proceedings of the 10th International Congress polluting effluent, smoke from a steam product. There is usually high demand for of Essential Oils, Fragrances and Flavors, generator (unless electrically powdered) good mulches in the horticulture, Washington DC. Amsterdam: Elsevier Science and the water distillate from the charge agriculture and home gardening sectors. Publishers, 1986: 415-24. bin. These effluents fall under the Other potential by-products from 5 Mookherjee BD, Trenkle RW, Wilson RA. Live vs. jurisdiction of local environmental distillation wastes include hydrosols from dead (Part II): a comparative analysis of the protection authorities. Smoke discharges certain distillate waters, although these are headspace volatiles of some important may require filters to trap excess carbon limited to a few crops like lavender, rose, fragrance and flavor raw materials. Journal of emissions and distillation effluent may and other florals. Spent foliage can be Essential Oil Research 1989; 2: 85-90. require aerobic or anaerobic treatment in used as cattle feed base, ferro-cement 6 Menage E, Nicholson K. Used oil as an a pond before discharge into the filler for green bricks and buildings, and as alternative boiler fuel- promises and problems, environment. a source of fuel for steam production in Southeastern apos; 93, Proceedings, Charlotte, the distillation plant. PC NC. IEEE, 4-7 April, 1993. Potential by-products from 7 For layouts and plans see: Dupont F. Essential the distillation process References oil extraction from herbs using solar energy – a The production of any possible by- 1 Clark RJ, Read C. Production of peppermint oil: thesis summary. http://www.uni-kassel.de/fb11/ products from the waste products of a model of best practice for Tasmania and agrartechnik/Fachgebiet/personal/Florent/ distillation, not only assists in the handling Victoria, Canberra. A report for the Rural Florent_Thesis_summary.pdf (accessed 7th of wastes, but in adding value to the Industries Research and Development January 2009). process through either savings or extra Corporation, August 2000, p61. 8 Munir A, Hensel O. Development of a solar revenue gained. 2 Hunter M. Essential oils: art, agriculture, distillation system for essential oils extraction The spent foliage of many plants after science, industry and entrepreneurship: a focus for herbs – Conference on Utilisation of diversity distillation can by utilised as mulch. Mulch on the Asia-Pacific Region. New York: Nova in land use systems: Sustainable and organic is very beneficial in weed control and Scientific Publishers, 2009: p417 approaches to meet human needs. Tropentag, maintaining moisture in the soil after rain 3 Matile P Altenburger R. Rhythms of fragrance , 9-11 October 2007. http://www.tropentag.de/ or irrigation. Using spent foliage as mulch emission in flowers. Planta 1988: 174: 2007/abstracts/links/Hensel_4GdqiE2W.pdf is also part of a sustainable farming 242-7. (accessed 7 January 2009). system and encouraged. Spent foliage 4 Mookherjee BD, Trenkle RW, Wilson RA, 9 Mateus EM, Lopes C, Nogueira T, Lourenco after oil extraction usually makes good Zampino M, Sanads KP Mussinan CJ. Fruits and , JAA, Curto MMJ. Pilot steam distillation of September 2012 P E R S O N A L C A R E 9