MONGANA

REPORT
ST
1 RIVISION

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 MONGANA REPORT COMPILED
Compiled by Ir. N. Ravi Menon

1. STERILISATION
As most of the mills in Malaysia appear to be poised for bunch crushing followed by
an additional stripping let us pause for a while and have a second look at some
fundamental and basic facts the MONGANA researchers have solidly established
from 1952 to 1955, which simply can not become obsolete during the passage of time.
The question to ask ourselves is- are we doing the sterilization the correct way with
the full understanding of the various issues involved in the process as when we look at
the Mongana report, the researchers do not seem to have missed out anything. The
only visible change after the report is that the pollination now is assisted by t he
weevils, which had improved the pollination efficiency leading to the formation of
more fruits in the bunch. This paper intends to examine some of the findings of the
Mongana Reprt in a chronological sequence.

The sterilisation process by heating the bunches was originated by Fiekendy, Annam
and Van Heurn and the initial objective was to inhibit the lipase activity in the pulp
that caused the hydrolysis of the oil. Very soon they recognised other useful effects of
wet or dry steam heating of the bunches. The application of this heat was found to
increase greatly the settling ability of the crude oil

In the early days, heat was applied as steam at atmospheric pressure, naked fire or hot
water and later steam under pressure became popular as the sterilisation cycle could
be made shorter especially when the crop started being processed as bunches instead
of loose fruits. With the advent of pressurised steam sterilisation becoming popular
for processing bunches other phenomena were observed. Heat not only affected the
lipase activity and the ability for the oil to settle but also the efficiency of the oil from
the digested mash, the recovery of the oil from the solids present in the crude oil, nut
breakage in continuous presses, the nut cracking efficiency and the oil bleachability
and other characteristics. The objective of sterilisation broadened considerably so that
it may be said that sterilisation is the precursor to all the subsequent processing
operations.

The effects of dry and wet heats

When dry heat in the form of hot air was used the desiccation of a ripe bunch failed to
induce the loosening of fruits even when kept in a furnace at 100 o for 128 hours.
They become brittle but do not shed fruits. An increase in temperature did not
improve the fruit detachment but had a pronounced impact on the colour of the fruit.
After three to four hours the dark red colour changed uniformly to brown. A slowing
down of the natural fruit abscission was noted in bunches stored in dry air at 50 o C to
60 o C.
The prolonged storage of fruit bunches under water at high temperature has the
property to split the fruit connection to the bunch, a property that was made use of in
the continuous sterilisation trials done at Mongana.

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Quarter bunches and spikelets stored at temperatures between 3 o C and -10 o C
remained firmly attached to the bunch, while the control bunches kept at an ambient
temperature of 28 o C stripped completely after 24 hours. Also samples lightly
sterilised for one hour in water at 45-50 o C did not strip at all but after 24 hours
stripped completely after 5 days, whilst the fruits of un-sterilised bunches kept at a
low temperature during the same period did not detach themselves from the bunch.
This indicates that the natural process of fruit abscission is of enzymatic origin and its
intensity decreases as the temperature departs from the ambient levels. It practically
comes to a standstill at 100 o C and 0 o C. The spikes immersed in hot water at
different temperatures and at different durations indicated that for a bunch soaked in
hot water at 90 o C stripped completely in 90 minutes, whereas at 100 o C and 110 o C
they stripped fully in 50 and 20 minutes respectively. It was found that the addition of
surfactants like caustic soda or alkyl-aryl sulphonate at 0.5% concentration levels
could accelerate the stripping process significantly.

The stripping of fruits from the spikes did not seem to involve difficulties since it only
required heating up the connecting tissues to 110 o C for approximately 20 minutes
and at 100 o C complete stripping was achieved in 45 minutes. The same was possible
by using steam at atmospheric pressure.

The artificial abscission process is found to be directly governed by the temperature

and follow the law: log t = K (T-T1)
Where, t is the time of sterilisation in minutes, T1 Temperature of sterilisation and T a
temperature approximately equal to 140 o C and the constant K=0.04.

Table.1 The Time vs Temperature to achieve 100% stripping

Temp o C 80 90 100 110 120 130 140

Time Min 250 100 40 16 8 2 1

If the same technique is applied to bunches instead of the spikes, the percentage of
stripping was found to be extremely low. The soaking of spikes in water at 100 o C
for one hour ensures rupture of all insertion points but if the same conditions are
applied to bunches the result is very high percent of hard bunches. The study of heat
transfer into the bunch indicates that the theoretical conductivity is extremely low.

For instance, the core of a 15 kg bunch kept in an oven at 100 o C reach a temperature
of 48 o C only after a dwelling time of 6 hours. If the temperature is 140 o C
corresponding to the saturation temperature of steam at about 2.6 barg (38 psig), the
core of an identical bunch reaches a temperature of only 51 o C after the same period
of 6 hours. The low thermal conductivity is inherent in the very nature of the bunches
and in the air occluded in them. The thermal conductivity of air is about 10 times
lower than that of oil and 30 times lower than water. Therefore it is important to
remove as much air as possible during sterilization and this can be done one of the
following: extraction, diffusion or displacement but in actual practice the last one is
found to be the most practical one.

The air extraction method consists in applying a vacuum either before sterilisation
proper or after the heating of bunches. But this was found to be very time consuming

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and moreover the sterilizer is designed as a pressure vessel rather than a vacuum
chamber and this poses some problems related to safety.

In the case of a small vertical sterilizer (1 t capacity) the theoretical time of diffusion
is about 10 hours but in a horizontal 7.5 tonne sterilizes, which provides a larger
surface of contact the diffusion time is shortened to about 3 hours. The straight
diffusion technique can not be applied to mix steam to a large volume of air in a
sterilizer with a view to expel them through the pressure release valves.

The displacement of air under the effect of steam may be complete in a vessel of large
dimensions. Steam is admitted slowly at the top of a horizontal sterilizer and the air
swept away from the sterilizer. It is actually possible to observe in a horizontal
sterilizer the door of which is open that the steam remains at the top and shows no
tendency to mix with air due to the marked density difference between the steam and
air: 0.598 g/dm3 for dry saturated steam at 100 o C against 1.043 g/dm3 for wet
saturated air at 50 o C. The compositions of the air/steam mixture determined
simultaneously at various points of the sterilizer after a short time of sweeping are
found to be as follows: 0.1 litre of air/ kg of steam at the top, 10.1 litres of air/ kg of
steam in the middle and more than 200 litres/kg of steam at the bottom.

In a sterilizer full of bunches the expelling of air by steam sweeping is slower and less
complete. It is practically necessary to maintain a continuous bleed off of steam
owing to the fact that the de-aeration of the bunches proceeds slowly and
progressively. In order to study the impact of de-aeration three trials were conducted
on a homogeneous batch of bunches. (a) The sterilizer was swept for 10 minutes and
the bunches sterilised for 40 minutes at 3 bar steam pressure with continuous bleeding
of 200 kg steam/hour.(b) No sweeping or continuous bleeding or condensate
discharge carried out and sterilised the same way (c) Triple peak sterilisation carried
out with neither sweeping nor steam bleeding.

The results were as follows: In (a) the bunches were completely stripped. In (b) 43%
completely un-stripped bunches and 20% partly stripped bunches. In (c) 4%
completely un-stripped and 28% partially stripped bunches. The Mongana researchers
summed up their observations which should serve the mill engineers as a very good
bench mark before they venture into any modifications of their sterilization system.

1. A 10 minute air sweeping with steam at the rate of 100 kg per hour expels 80
to 90% of the air from the sterilizer.
2. After the steam sweeping the air content of the steam is limited to 0.2 litres
per kg of steam.
3. During the first pressure build up and during the pressure release, some de-
aeration takes place as a result of the condensate discharge that expels 9 to
18% of the total air.
4. During the second and third pressure build up 1-5% of the air will still find its
way out provided the preliminary sweeping was effectively done.
5. If, after the pressure release, the pressure is maintained at the atmospheric
level, the de-aeration increases slightly during that period and after a period of
time5 to 15 minutes the steam condensates through cooling causing some
external air to be sucked in.

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 6. It is not possible to assess the efficiency of air removal without carrying out at
least a semi quantitative determination of the air content of the steam. This is
an important point to remember. The assessment is done by drawing out a
certain amount of steam, weighed and condensed. Simultaneously the air is
also measured.
7. The de-aeration of bunches stakes place only after they have been heated up
for some time at high temperature. It is useless to try and improve the de-
aeration by prolonging the steam sweeping of air at atmospheric pressure.
8. It is essential that there is a continuous discharge of air laden steam during the
whole sterilization cycle.
9. For complete displacement of steam the steam must be admitted slowly into
the sterilizers.

The Effect of Temperature.

The efficiency of stripping depends not only on the time reached during a sterilization
cycle but also the duration the temperature was maintained. In practice, it was
observed that with an adequate sterilization regime it takes an hour for the bunch core
to reach a temperature of 130 to 135 o C. For satisfactory conditions of heat
penetration after efficient de-aeration , the time during which the temperature is
maintained above
100 o C should not be less than 35 minutes even when the temperature attained is 130 o
C.
It is possible for the steam temperature to exceed the saturation temperature of the
incoming steam due to the effect of wire drawing that superheats the steam. When
saturated steam at a pressure of 5 -6 barg is throttled to 4barg the steam will tend to
superheat and the temperature may rise to 148 to 150 o C instead of remaining at the
saturation temperature of 143.6 o C.

The Effect of Pressure.

The rate of heat penetration into a bunch is proportional to the temperature difference
between the steam and the bunch and not the pressure and as such a higher steam
pressure will not be able to shorten the sterilization cycle as for example the
temperature difference of steam between steam at 3 barg and 4 barg is ( 151.8-143.6 =
8.2 o C ) is not significant enough to cause a dramatic improvement in sterilization
efficiency. In addition the disadvantage in the indiscriminate increase of steam
temperature is the reduction in the DOBI value of CPO. A decrease in the sterilization
pressure must be compensated by an increase in the time of sterilization. If the
sterilization time needed is 25 minutes at 3 bar and if the pressure is reduced to 1.5
bar, the sterilization time must be extended by 30 minutes making the total
sterilization time 55 minutes to achieve the same stripping efficiency as with the
higher pressure.

Sweeping Operation

Since the density of steam is lower than that of air, the steam required for the
displacement of air must be admitted into the sterilizer form the top to the bottom.
Also the sweeping must be effected without creating eddies in the sterilizer as that

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would impair the complete evacuation of the air and/ or would increase the steam
consumption.

Theoretically, the ideal shape for de-aeration by displacement is the vertical cylinder
and in practice vertical sterilizers closely conform to that shape and can effect good
de-aeration provided that the steam is admitted at a relatively low rate into the dome.
In a horizontal sterilizer fitted with only one steam inlet, the de-aeration takes longer
time and also not complete. But with multiple steam inlet points the performance can
be brought to the same level as the vertical units.

Whatever the cycle, long or short, single or multiple peak , it is always an advantage
to ensure the evacuation of most of the air by sweeping it from the top to the bottom
by the incoming steam.

The first pressure release may be of relatively short duration of 3 to 4 minutes during
which the air is swept out of the sterilizer by the steam but the intermediate pressure
releases are performed after diffusion of steam into air. It is therefore necessary to
allow diffusion to take place and to avoid blowing down after an extremely fast
pressure build up as diffusion requires certain time to be effective.

Effect on oil extraction

As a result of the ageing of the fruit, the oil bearing cells appear to acquire a special
permeability, which leads to unimpeded oil flow. The permeability eventuates at any
temperature of sterilization, but in addition, high temperature induces the breaking up
of the cells. The result is that upon digesting aged fruit sterilized at a temperature
lower than 100o C a large flow of almost pure oil, so called ‘Virgin Oil’, will be
observed. At a temperature higher than 100 o C and for a longer time of sterilization,
cells or cell debris will find their way into the crude oil during d igestion. The
weakening of the intercellular cement which causes the breaking up of the cells may
be due to liquefaction, solubilisation, hydrolysis and etc. It increases the intensity as
the temperature rises but remains negligible as long the temperature does not exceed
98o C and is not maintained for more than 20 minutes.

It was observed that the sterilization process done under pressure leads to a higher
loss of oil on nuts in addition to increased oil losses in the fibre than when done at
atmospheric pressure (during centrifugal extraction). Sterilization done under pressure
indicated a sharp increase in dehydration when compared to sterilisation at
atmospheric pressure(30%). This moisture loss during sterilisation under pressure is
equally distributed in fruits, spikes and the stalk. Life steam at atmospheric pressure
does not seem to have a marked effect on the moisture content of the fruit bunches.
The desiccation occurs abruptly when the steam is blown off and during sterilisation.
Exposure of the fruit to air after the blow off also contributes to the loss of moisture.
The quantity of moisture evaporated is closely related to the temperature. The volume
removed has a limit called the limit of desiccation (approximately 20% moisture)
after which no more moisture can be evaporated even by repeated sterilisation. This
contradicts some elementary principles as when the steam pressure is reduced
abruptly like during blow off the bunches are expected to shed a portion of its
moisture. The assumption is that the bunches re-absorb from the steam the moisture it
lost during the blow off or during the pressure build up to restore the equilibrium.

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This point is important as it is customarily acknowledged that the oil extraction,
especially by the press, is affected by the degree of de-hydration of the fruit even
though on industrial scale this could not be confirmed.

In general, the heat penetration was found to be directly linked to the efficiency of oil
extraction up to a certain limit beyond which an equilibrium is established between
the capillary forces retaining the oil and the applied mechanical forces to extract it.
The heat penetration acts on the tissues connecting the fruit to the stalk and also has a
marked effect on oil extraction efficiency.

Stripping and oil extraction efficiency are closely related. If the stripping efficiency is
low the oil extraction efficiency is also likely to be low and double stripping does not
address the real problem other than recovering the fruits lost in un-stripped bunches.
This indicates that when stripping is not efficient, sterilisation is the culprit. Rectify
this and all other problems are addressed in one go.

Multiple pressure build ups and releases has a detrimental effect if it entails a drop in
the average temperature in the sterilizer or in the fruit, which happens when the
repeated pressure releases reduce the time of contact between the steam and the
bunches despite a continuous increase in sterilizer temperature in the initial stages.
Then temperature profile for a sterilisation cycle with 7 blow downs after the 20 th to
the 40th minute gets through a plateau and the contact heating time (21 minutes at
above 100o C ) will be significantly less than that recorded (28 minutes) for a cycle
without any blow down at all. With one blow down the contact time was 40 minutes.

Impact on nuts

There is no doubt about the fact that a freshly de-pulped nut cracks under the effect of
a blow and as the shell and the kernel are bound together in the fresh nut the cracking
of the shell necessarily means the cracking of the kernel as well. The nut cracker
machinery designers should always remember this basic principle when they design
nut crackers. The desiccation of nuts separates the shell from the kernel. It is
generally believed that the cracking can be efficient only on nuts with a moisture
content of 7.5% on nuts and 12% on kernel. But if the fruits are well cooked using
triple peak sterilisation, wet nuts with 15% moisture in nut and 20% moisture in
kernel also can be cracked with 98% cracking efficiency. The cracking efficiency
depends a great deal on de-aeration as can be seen in the following table.

Table: The Effect of different sterilization regimes on Nut cracking efficiencies

With de-aeration Without de-aeration

Blow down > 30 seconds

Cracked nuts 98.2% 56.2%
Split nuts 0% 16.5%

Without blow down

Cracked nuts 89.0% 37.9%

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Slit nuts 0.7% 4.4%

The two results indicate that the de-aeration process reduces the percentages of un-
cracked nuts significantly. The de-aeration and steam bleed off technique affect not
only the proportion of un-cracked nuts but also that of broken kernels.

Nut breakage

Nut breakage is considerably reduced by pressing the fruit at a temperature close to

100o C. But if the bunches are sterilized at atmospheric pressure and then
heated up to 100o C during pressing nut breakage is more pronounced than when it is
subjected to triple peak sterilisation and heated to 100o C during pressing. This is due
to the shrinkage of the kernel caused by the penetration of heat into the core of the
kernel that also allows the shell to undergo greater deformation. Wet kernel does not
appear to offer great resistance to pressure and torsion. They certainly do not resist the
kind of pressure that may be applied to the nuts without breakage. This may be
explained as follows. Fruits sterilised with live steam at atmospheric steam is heated
up and pressed hot. After a period of rest the nuts are cracked. In that case, nuts with
no apparent damage yield broken kernels the appearance of which indicates that the
kernel splitting occurred before the cracking operation. The kernel still sticking to the
shell was therefore crushed open although the more elastic shell resisted cracking
perfectly. Adequate sterilisation therefore frees the kernel from the shell and allows a
more important deformation of the latter without the risk of kernel crushing.

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Impact of Sterilization

In the last paper we discussed the underlying principles involved in the

sterilization process. Proper sterilization has a profound influence on the kernel
recovery in terms of the extraction rate as well as the kernel quality. The minimum
sterilization temperature of about 130o C was not arbitrarily chosen but arrived at after
exhaustive trials and sound research by Mongana scientists in 1952.

Effect of Desiccation

The study on the relationship between the desiccation of the pulp and its
resistance indicates that for fresh pulp the resistance to pressing is 5-6 bar and it
drops to 2 to 3 bar after autoclaving for 10 to 60 min and with further intense
desiccation and a moisture level of 7% the resistance rises back to 5 bar.

Solubility of bunch components

Before sterilization, the stalk contains about 23% of the soluble matter but
after triple peak sterilization, the soluble fraction increases to approximately 26.5%.
The sterilizer condensate would contain about 3% of the soluble NOS. The mills are
urged to conduct trials to establish these values from the sterilization condensate and
the NOS measurement for different sterilization cycles. However, care should be
exercised to account for the insoluble NOS like sand and fibrous material etc.

Absorption of Oil by the Stalk

During sterilization, some oil will be expelled from the fruits and a portion of
which will find its way into the sterilizer condensate whilst the remainder will be
absorbed by stalks, the spikelets and the calyx leaves. Perhaps the millers can
appreciate the need to reduce as much of the stalk as possible to reduce this
unrecoverable loss. As much as 10% of the total oil contained in loose fruits will be
expelled during the sterilization process. The fresh loose fruits collected by the estates
also will shed oil during triple peak sterilization but to a lesser extent than fruits
detached through ageing. Simply said, this means that theoretically loose fruits
should never be mixed with fresh bunches during sterilization - although this may be
difficult in practice. It also appears that old bunches should be separately sterilized
from fresh bunches if oil losses are to be reduced at all areas. It should be noted that
50% of the fruits detach from the bunches when they are dumped on the thresher
hopper.

A long sterilization cycle or a higher sterilization pressure do not seem to

affect the oil absorbed by the stalks. The oil content of sterilized empty fruit bunches
varies from 0.4% to 1% to on wet basis, the corresponding values being 1.2% to 3%
on dry basis. The oil content of the outside layer (spikelets) may reach four times that
of the core (rachis). After stripping the oil content rises appreciably to 3% on wet
basis and 7% on dry basis. These values vary widely from bunch to bunch and it is
difficult to obtain an acceptable average value. The fruits on the outer layers of the
bunch are softer than the fruits on the inner layers and as such the former are more
prone to shed oil.

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 The amount of oil absorption by the stalk also vary with the type of
equipment used for stripping the bunches. In Mongana, trials were also conducted to
compare the oil contents in stalks using the drum stripper as well as the beater arms
after separating out the self-detached fruits. The stalks from the drum stripper had 5%
oil content compared to beater arm which only had 3% on dry basis. However, the
Mongana report says that the trials had several flaws affecting the validity of the
findings.

The thickness of the bunch layer within the sterilizer and their position exerts
a marked influence on the oil absorption by the bunches. If the layer thickness is 2 m,
the difference between the oil absorptions of the top and bottom layers was found to
be 1%. As the sterilizer cages are becoming bigger and bigger as is the trend today in
palm oil mills, do not forget that the increase in cage height would introduce higher
oil losses in empty fruit bunches.

Two batches of sterilized bunches, one after cooling down for a period of 12
hr and the other reheated for 10 min after the same period of cooling down and
subjected to stripping showed no increase in the oil content of the empty fruit bunches
except in the oil content of the bunches located at the top and the bottom that showed
significant variation in the latter.

Stripping of Unripe Bunches

It is often said that the hard bunches can never be stripped no matter what
sterilization regime is adopted. This was investigated at Mongana. Their findings are
that no bunch, as green as it may be, can resist a good sterilization like the triple peak
sterilization with sweeping of air and continuous steam bleed off. In the Mongana
trial, unripe bunches (8 days before maturity) were harvested and they were separately
sterilized and stripped and 99% to 100% of them stripped completely. Mongana
finding fail to support the notion that double stripping is an essential requirement for
successful stripping of the bunches clearly indicating that the millers are fighting the
consequence rather than the cause.

Steam Consumption

The minimum steam consumption per tonne FFB for a simple sterilization was
found to be 190 kg at barg steam, pressure. For triple peak sterilization without steam
sweeping and continuous bleed off the steam consumption ranged from 200 to 240 kg.
The steam sweeping and continuous bleed off required an additional 50 to 100 kg of
steam giving an average consumption of about 300 kg steam t -1 FFB. The distribution
of the steam consumption were: (a) 80 to 120 kg for heating up the sterilizer, average
33% (b) 120 to 140 kg for sterilization, average 43% and (c) 50 to 100 kg for
sweeping and steam bleed off, average 24%.

Continuous Sterilization
The Mongana report says that there are no obstacles for continuous sterilization under
constant steam pressure and theoretically nothing could rule out the construction of
bunch conveyors which would enter pressure chambers through air locks. Mongana

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suggested the use of three conveyors and chamber units for a triple peak sterilization.
As this system could be costly, Mongana suggested a different approach. The fruit in
the spikelets soaked in water at 100o C for approximately 1 hr-1 was found to strip
completely but fruit in bunches treated in the same manner refused to strip at all. This
was found to be due to the difficulty in heat transmission within the bunch caused by
air insulation. It was also observed that soaking of bunches in water under a pressure
of 1.5 bar-g for 90 min led a stripping efficiency of 98%. It was also established that
the addition of surfactants allows a faster de-aeration of the bunches and improved
heat transfer.

Based on the above findings, Mongana attempted the design of a continuous

sterilizer. It comprised a giant size 10 m high U-tube into which bunches were fed.
Hot water from the top of the tube was drawn and passed through two heat
exchangers and pumped into the bottom of the U-tube. The pressure at the bottom of
the tube was 1 bar-g with the boiling point of water at 120o C and the temperature of
the water at the top at 98o C. The bunches moved through the column by a 22 m long
chain conveyor. The sterilization time for this system required a resident time of 2 hr
and 45 min for efficient stripping. The fruit also was found to be hard necessitating a
longer period of digestion and the digested mash had a different appearance. Nut
cracking also gave unsatisfactory results. However, the cracking was more effective
on nuts derived from fruits sterilized with steam at atmospheric pressure than when
done with hot water. In summing up, Mongana declared that a continuous sterilizer
working on the concept of water columns can be designed as it would lead to
satisfactory stripping but further research work will be needed to address the problem
of fruit processing.

Sterilizers are classified into two types: vertical and horizontal ones. Whilst most of
the millers are familiar with the horizontal sterilizers, they will have to contented with
the pictures of the vertical ones as there are no vertical operating units in Malaysia.
The vertical sterilizers with capacities ranging from a few hundred kg to five tonnes
are filled up directly or sometimes receive a basket loaded with bunches. Most of the
young palm oil mill engineers in Malaysia probably never had a chance to actually see
a vertical sterilizer. The same applies to the hydraulic presses that have virtually
vanished from Malaysia.

It will be worth while to establish a palm oil processing machinery museum to benefit
the future generation of millers as the old designs can certainly come back with
modern features. Now the vertical sterilizers are coming back and some Malaysian
entrepreneurs have already built and installed them overseas as there are demands for
small mills in the range of 5 to 10 tonne ffb h -1 capacities in Africa and Latin
American nations. The vertical sterilizers maintain the same steam pressure as the
horizontal units and use the conventional processing methods for both oil and kernel.
It is still a batch process well suited for processing fruits from a 1,000 to 1,500 ha
estate having a yield of 15 t h-1 y-1 , that is normal in many countries.

Vertical Sterilizers

In the old version of the vertical sterilizers the loading takes place through the top
mostly by means of a bucket elevator. In the case of sterilizers with large capacities,

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as bunches fall from a height of several meters bruising can not be avoided even if a
damping cushion is provided. Unloading is labour intensive and may take about an
hour as it is difficult due to the compaction of bunches during sterilization. The
thickness of the ffb layer is high, oil losses in the EFB is particularly high. In this one
tonne of bunches occupy approximately 2 m3 of space as there is not much unused
space in a vertical sterilizer. The vertical sterilizers have high thermal efficiency and
the weight of metal to be heated up in relation to that of the bunches is also very low.

The basket vertical sterilizer makes it possible to empty the baskets by tilting them
around fulcrum points placed near the centre of gravity or though the bottom. A
system to extract the basket from the sterilizer like monorail, gantry etc. will be
necessary. The basket capacities ranges from 1 to 3 tonnes of bunches . The unused
space in this sterilizer is slightly more than the previous type.

Horizontal Sterilizer

In horizontal sterilizers the unused space is large and the corresponding ratio of the
weight of the metal to that of the bunches leading to a higher consumption of steam.
Oil loss in EFB is lower than in a vertical sterilizer as the bunch layers are not very
thick. The loading of ffb in and out of the sterilizer is fast and easy especially now
with the double door type. The de-aeration however, is better in the vertical sterilizer
but with continuous air bleeding the air purging efficiency can be improved.

Recommended Design Criteria for Sterilizers

1. The ratio of the weight of the metal to the weight of bunches should as low as
possible.
2. It must be possible to open the doors in a minimum of time.
3. The closing device must be simple and sturdy. It must be designed so as to
ensure that the steam tightness is maintained as long as possible and the gasket
replacement is easy. The material used for the gaskets must be lasting. In the
horizontal units the gaskets should be preferably sunk in the door rather than
in the body of the sterilizer because in the latter case the gasket is frequently
damaged as a result of the movement of overfilled or carelessly filled cages.
If the gasket is sunk in the sterilize it must be protected against the impact of
bunches which may cause the damage.
4. The height from which bunches drop into the cages during the loading should
be kept to the minimum.
5. The injection of the steam into the sterilizer can be made at a single point
located at the top in the case of vertical sterilizers. For the horizontal ones,
multiple inlets preferably connected to a steam manifold extending over the
whole length of the sterilizer are essential.
6. The steam inlet pipe must be so sized as to get 3 bar-g pressure inside the
sterilizer within 10 minutes. The steam requirement at the beginning of the
sterilization cycle is high and the pipe sizing should be based on a steam flow
rate of one tonne of steam per tonne of the bunch during the initial steam flow.
7. The pressure reducing valve must not close gradually as the pressure rises in
the sterilizer. It must cut off steam supply when the steam pressure nearly
reaches the required level.

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 8. The steam exhaust valve must be located at the bottom of the sterilizer. The
diameter of the pipe must be large enough to complete the steam blow down in
4 minutes when all the bunches have reached the temperature of the steam
(about 140 o C)
9. During the sterilization, all the condensate must be evacuated through a steam
trap fitted with a filter that can be easily cleaned or through a valve, the setting
of which must be ascertained by trial and error.
10. In addition to discharging the condensate a continuous bleed off of steam from
the bottom of the sterilizer must be provided. The bleed off valve may be
fitted to the bottom dished end in vertical sterilizers or a manifold extending
over the whole length of the vessel in the case of horizontal ones.
11. The sterilizer control equipment consists of a dial pressure gauge, a pressure
recorder and a clock. A temperature recorder indicating the temperature at the
bottom of the sterilizer is also useful. During commissioning a sterilizer it is
useful to make use of an apparatus to determine the air content in steam with a
view for selecting the appropriate sterilization cycle.
12. A horizontal sterilizer may have a slight slope in order to facilitate the
introduction of cages, the discharge of the condenser and the de-aeration
through sweeping.
13. The exhaust steam may be used for the sweeping of air. In that case, the
sweeping must be prolonged to compensate for the less heat content in the
steam than the fresh steam.
14. The sterilizer must be lagged.
15. The sterilizer must be fitted with the usual safety devices used on boilers and
also with s door locking device operating as long as the vessel is under
pressure. They also must be fitted with a standard flange for connection to a
calibrated pressure gauge.
16. The condensate must be drained adequately.
17. A silencer may be installed on the exhaust line.
18. The valves operating wheels must be grouped in a control post so that
automation to achieve any type of cycle can be easily arranged.
19. The sterilizer bay must be located away from the main process building so as
to avoid the leaking into process plants and machinery.
20. The steam consumption is not steady throughout the sterilization process. At
the beginning of the pressure build up, allowance must be made for large
steam requirements like one tonne of steam per hour per tonne of bunches.
After a few minutes they fall off considerably and do not exceed 50 kg per
hour per tonne of bunches towards the end of the cycle. The total steam
consumption is approximately 250 kg per tonne of bunches. These indications
permit to ascertain if the average hourly capacity of the boilers is sufficient
and moreover, to establish if the boilers can cope with the sharp steam demand
at the beginning of the sterilization. A steam accumulator may be the answer
to the problem of achieving steady steam draw off from the boilers.

2. EXTRACTION PROCESS
The extraction process can be generally classified under two groups.
(a) Dry extraction process
(b) Wet extraction process

13
In the dry extraction process the ratio of nut to pericarp in the fruit plays an important
role. The study of dura, tenera and other crossed derivatives shows the following
characteristics in terms of this important ratio.

Table 1. The Pericarp to nut ratios of different Tenera crossings

Types % Pericarp % Nuts Ratio of pericarp to nuts

Pure Dura 40 60 0.7 / 1
Dura x Tenera 60 40 1.5 / 1
Tenera x Tenera 65 35 1.9 /1
Dura x Pisifera 75 25 3 /1
Pure Tenera 80 20 4 /1

Even though a Dura x Pisifera crossing should theoretically yield 100% Tenera, in
actual practice there will be some pure Dura in the crossing amounting to 5% to 10%.
The Table 1 shows that the ratio of pericarp to nuts in pure Tenera is 6 times that of
pure Dura.

The ratio of fibre ( fibrous residue of the pericarp after the extraction of oil) to nuts
for the different crossings remains identical even after the extraction of the oil from
the pericarp as the ratio of fibre to pericarp in all cases remains constant at 2/3.

During the extraction process, not only the oil is removed from the pericarp but part
of the pericarp termed non-oily solids as well as part of the moisture. Assuming 70%
of the pericarp is removed during the extraction process, the pericarp (now called
fibre) would have the following composition (30%) shown in brackets:

14
 Table 2: Ratio of fibre to nuts after oil the extraction

Types % Pericarp (fibre) % Nuts Ratio pericarp/(fibre)

to nuts
Pure Dura cake (Congo) 40 (12.0) 60 0.7 (0.2)
Dura x Tenera cake 60 (18.0) 40 1.5 (0.45)
Tenera x Tenera cake 65 (19.50 35 1.9 (0.56)
Dura x Pisifera cake 75 (22.50 25 3 (0.9)
Pure Tenera cake 80 (24.0) 20 4 (1.2)

The new fibre to nut ration would is shown in brackets. The portion of the pericarp
viz: oil, moisture and non oily solids finding its way to the crude oil during the
mechanical extraction process ranges from 65% to 75% and depends on the types of
extraction process involved.
Table 2 shows that the ration of the ratio of fibre to nuts in the Dura cake from palm
grove bunches is only 1/5 of the cake but in pure Tenera cake this ratio exceeds 1. The
cake has obviously more fibre than nuts.

If the nuts are graded using a screen with 18mm perforations, the nuts retained by the
screen are likely to be Dura, while those passing through will have a high percentage
of Tenera. The apparent densities of different types of nuts were found to be as
follows:

Density: Dura : 781 kg/M3 Tenera : 656 kg/M3

The “free” volume between nuts on the but or interspaces were determined by filling
up a known volume of nuts with water and they were found out to be as follows:

Void between nuts: Dura: 563 M3 /kg Tenera : 832 M3 /kg

The density of the digested pericarp is 925 kg/ M3 . From the value of the free space
and the density of the filling medium (i.e.water = 1000kg/M 3 ), it is possible to
ascertain the mount of pericarp necessary to fill up the void by multiplying the free
space by 0.925. Hence for every kg of nuts the following weight of mashed pericarp
will be necessary for filling up the void between nuts for establishing equilibrium.

Weight of pericarp to fill the voids: Dura: 0.521kg Tenera : 0.770 kg

At this point of nut/pericarp equilibrium when the voids are completely filled up by
mashed pericarp, the composition (expressed in weight) of the mixture will be as
follows:
Table 3: Ratio of Pericarp to Nuts at equilibrium

Typs Nuts % weight Pericarp % by weight Ratio- Pericarp/ Nuts

Dura 65.7 34.3 0.5
Tenera 56.5 43.5 0.8

15
Table t gives the composition of various types of fruits. It shows that the ratio pf
pericarp to nuts is 0.7 in Dura fruits and in excess of 1.5 in the crossings. Despite this
there will always be an excess of pericarp in the digested mash leading to a dispersion
of nuts in pericarp. Consequently, nuts will be distributed in the pericarp without
mutual contact.

During the extraction of the oil from the mash, as the oil is removed, there will be an
increase in the density of the pericarp as effectively the pericarp is converted into
fibre at the end of the process. The density of this low oil content fibre determined
under pressures of approximately 1 bar and 8.3 bar were found to be 1.01 and 1.04
kg/M3 respectively. The pressure prevailing at the periphery of a centrifuge basket of
1.2 metre diameter revolving at 1,00 rpm is approximately 10 bar ( 145 psig) and the
pressure prevailing in the continuous screw pressing process is approximately 85 bar
(1,232 psig). In the latter case a significant portion of the non oily solids will find its
way into the extracted oil. Two cases may be considered: (a) An extraction process
during which 60% of the pericarp is recovered and another (b) in which 75% of the
pericarp is recovered.

Table 4 : Variation of fruit components during oil extraction

Removal of 60% of the pericarp Removal of 75% of the pericarp

Dura (kg) Tenera (kg) Dura (kg) Tenera (kg)
Initial pericarp 40 80 40 80
Initial nuts 60 20 60 20

Fibre after oil extraction 16 32 10 20

Void between nuts 0.034 M3 0.017 M3 0.034 M3 0.017 M3
Wt. of fibre to fill voids 34 17 34 17

Fibre availability
Excess - 15 - 3
Deficiency 18 - 24 -

It can be observed that in the case of the Dura fruits there is always a deficiency of
fibre whether extraction is carried out by gentle pressing as in the case of centrifugal
basket or by high pressure pressing like screw pressing. By contrast in the case of
Tenera fruits, there is always an excess of fibre after extraction regardless of the
nature of the extraction process.
Theoretically, at the end of extraction all Dura nuts are in contact with each other
whilst the free space between them is incompletely filled up with fibre. In practice, a
large number of nuts are likely to be in contact with each other. On the contrary,
Tenera nuts are unlikely to be in contact with each other, on the average, the nuts
could be uniformly distributed in the cake without mutual contact.
These considerations indicate that an uniform pressure applied to Dura cake exerts
itself on the nuts, whereas on the pressure on Tenera cake exerts itself on the fibre.

It is possible to calculate, as has been done in Table 4, the initial pericarp content for
an extracted cake in which there is no excess or deficiency of any of the constituents.
The calculations shows that equilibrium occurs when the pericarp content of the
fruits is just above 60% in centrifugal extraction process in which 60% of the pericarp

16
is removed.. In continuous screw pressing in which 75% of the pericarp is removed
equilibrium occurs when the pericarp constitutes 75% of the fruit.

When bunches are processed instead of fruits, the material fed into the digester
contains impurities to the extent of 10% to 20% by weight of the fruit. These
impurities can be assimilated to the pulp. On completion of extraction they have the
same density as the fibre and the apparent composition. The diagram remains
therefore valid for bunches but the equilibrium simply shifts to the right. For instance
detached fruits containing 60% of pericarp are similar to fruit laden with impurities
containing only 55% of pericarp.

A fair number of observations confirm that there exists an optimum composition for
the centrifugal extraction process as well as extraction by continuous pressing. These
will be discussed in the next article.

17
 Dispersion of nuts on fibre Dispersion of fibre on nuts

DxP P.S
TxT DxT
Extraction: 60% of
pericarp without dirt
Zone of pulp
surplus

Zone of pulp difeciency

Extraction: 75% of
pericarp without dirt
Extraction 60% of
pericarp without dirt

Optimum

100 70 60 50

100 75 50 25 % Tenera

26 Oil on dry fibre

C: P.S.
24

22

20
A: Pure Pericarp

18

16 B: TxT

14
Oil on fibre corresponding to the
12 optimum with points A, B &C criteria

10

Continuous Screw Press Extraction .

18
This system of extraction was tried out on five different presses. All were screw
presses but three of them had coaxial screws revolving in opposite directions. The
other two had parallel screws. The capacity of the presses ranged from 1.3 to 9.6
tonnes of digested mash per hour (corresponding to 2 to 14 tonnes FFB per hour. The
power consumption varied from 2.2 to 11.2 kW. The finding were as follows

Advantages:

➢ Automatic operation
➢ High rate of extraction
➢ Low & steady power requirement
➢ Small floor space requirement in relation to capacity.
➢ Well extracted, dry cake , which can easily be separated into fibre and nuts.

Disadvantages:

➢ High nut breakage

➢ Restricted settling ability of the crude oil requiring the use of centrifugal
clarification.
With the screw press approximately 75% of the pericarp of the fruit finds its way into
the crude oil compared to 65% for the centrifuge. Therefore for this process high
percentage of pericarp is essential. In the case of fruit with low pericarp content, there
is not enough fibre at the end of pressing to fill up the space between nuts and as a
result the pressure is applied to the nuts rather than the fibre causing nut breakage and
the nut debris eventually occupy the free space between nuts. For normal D X P
bunch (pre-weevil period) the pericarp to fruit ratio was more than 65% or even
higher than 70%, if calyx leaves and other extraneous matters are included.

Food for thought

The pericarp to fruit ratio has now come down to 50% -55% indicating that the
screw presses used in our mills are no more well-suited for pressing the current
digester mash, unless high nut breakage is of no concern to the millers.
Theoretically, this would mean that the addition of some fibre or shell to the
digester mash to increase the pericarp to fruit ratio to 65% should improve the oil
extraction process with minimal nut breakage. Any mill willing to try this out?
Comments form millers are most welcome.

19
3. FACTORS AFFECTING EXTRACTION EFFICIENCY
Only one factor, the temperature of the digested mash, assumes real importance. It
affects the oil extraction form the cake and nut breakage. The temperature is linked to
viscosity. The crude oil from the press is extremely thick. An increase in temperature
lowers its viscosity and accelerates its extraction form the cake. The heating up of
fruit in a steam jacketed digester not fitted with a digester liner leads to a relatively
swift rise in temperature compared to a digester provided with a wear plates. The
fastest process is the injection of live steam that gives the best heat transfer efficiency.
The condensation of the injected steam does not affect the viscosity of the mash or the
extraction efficiency.

Continuous presses of low capacity yield a cake containing as little as 4% on dry fibre.
In the case of large capacity presses the losses do not fall below 7-8%.
The pressing of fruit at high temperature like 100o C appears also to improve the
removal of oil from nuts. At industrial scale, oil contents of 0.25% on nut have been
observed. The composition of crude oil is contingent upon the applied pressure: the
higher the pressure, the higher the cellular debris content of the crude oil. The millers
are urged to note this as a number of mills use extremely high press cone
pressures( even 90 bar-g) without realizing its detrimental effect on processing. The
solids generated by pressing will go into the crude oil and these solids absorb oil
resulting in higher oio losses.

The coaxial screw presses yield crude oil containing less non oily solids. At the outlet
of the press, the composition of the crude oil varies with the degree of oil extraction
from the cake; as the oil content of the latter decreases, crude oil shows increased
tendency to take the form described as vermicular sludge” containing approximately
20% oil and 20% dry matter. The composition and morphology of continuous press
fibre differ appreciably from those of the fibre from centrifuges and non-continuous
presses due to its low cellular debris content and high content of fibrous strands. The
occurrences of lumps of cellular debris observed during passage of oily and wet cake
through the de-pericarper is extremely rare with the continuous press cake as result of
the migration of a large proportion of the cellular debris into the crude oil. It is of
interest to note that the screw press can deal with poorly digested fruit. It is also
possible to extract as much as 60% of the oil without any digestion at all.

The test results on a small press with a capacity of 2 tonnes per hour are given in
Table 1. The crude oil was diluted with 50% water, filtered through a vibrating
screen and directly subjected to a centrifugal separation in a centrifuge. The recovered
oil was dried. All these operation were continuous. In the computation of the
efficiency, the losses in the bunch refuse and in the sterilizer condensate were not
taken into account.

20
 TABLE 1: OIL LOSSES IN CONTINUOUS PROCESSING

Component Test no.1 Test no.2

Oil in sample % to FFB % to total Oil in sample % to FFB % to total oil
% oil %
Fibre 3.77 0.58 2.42 3.33 0.51 2.03
Nuts 0.56 0.07 0.28 0.51 0.05 0.20
Effluent 0.67 0.41 1.72 0.57 0.42 1.65
Oily solids 2.91 0.14 0.57 2.21 0.11 0.45
EFB(est) 2.5 0.55 2.25 2.70 0.60 2.36
St.Cond (est) 0.1 0.02 0.10 - 0.02 0.10
Total - 1.77 7.34 0.1 1.71 6.80
Efficiency 92.66 93.2

21
 4. FACTORS AFFECTING NUT BREAKAGE

It will be interesting to study the continuous press material balance given in the
Mongana Report. This is reproduced here on two samples of D x P material.

1.Weight of FFB 210.925 kg 45.212 kg

2. Wt. of pure oil recovered 47.287 kg 10.675 kg
3.Oil Extraction Ratio 22.42% 21.61%
4. Wt. of Sterilized fruit including impurities 138.057 kg 29.582 kg
5. Ratio of S.F incl. impurities to FFB 65.3 % 65.4 %
6. Oil on impurities 10.26 % 11.21 %

Oil Losses

A. Fibre

1. Weight of fibre 32.323 kg 6.973 kg

2. Oil loss in fibre 3.77 % 3.33 %
3. Oil loss 12.124 kg 231 kg

B.Nuts

1. Weight of nuts 24.880 kg 4.551 kg

2. Oil on nuts 0.56 % 0.51 %
3. Oil loss 139 kg 23kg

C. Effluent

1. Weight of Effluent 128.724 kg 28.268 kg

2. Oil on Effluent 0.67 % 0.67 %
3. Oil loss 862 kg 189 kg

D. Oily Solids

1. Weight of oily solids 9.790 kg 2.338 kg

2. Oil in oily solids 2.91 % 2.21 %
3. Oil loss 285 kg 52 kg

Total oil loss 2.505 kg 497 kg

Overall efficiency 0.950 % 0.956 %

D x P Bunches: Analytical results and losses

22
 SAMPLE 1 SAMPLE 2
ANALYSIS OF Oil content Loss to Oil content Loss to
LOSSES in the FFB in the FFB
product product
Fibre 3.77 % 0.58 % 3.33% 0.51%
Nuts 0.56 % 0.07 % 0.51% 0.05%
Effluent 0.67 % 0.41 % 0.57% 0.42%
Oily solids 2.91 % 0.14 % 2.21% 0.11%
Bunch refuse(estimate) 2.5 % 0.55 % 2.70% 0.60%
Sterilizer condensate 0.1% 0.02 % -
0.1% 0.02%
Total - 1.77% - 1.71%
Efficiency 92.66% 93.20%

(b) Palm grove fruit

The fruits from palm grove bunch cannot be processes in a continuous press because
of the insufficient fibrous material in the bunch.

If an attempt is made to treat the fruit in a screw press in such a manner as to

obtain satisfactory oil extraction ,a portion of the nuts gets crushed thus making up
for the fibre deficiency.

It has been established in this report earlier that the deficiency in pulp ranges between
18 and 24 % by weight of the Dura fruit, according to the extent of the migration of
the pericarp into the crude oil.

Nut breakage is theoretically, likely to stop when the deficiency in fibre is

compensated by the formation of an adequate padding made of broken nuts.

This explains why nut breakage in the processing of palm grove fruit is not absolutely
linked to the degree of oil removal from the cake. For instance, the oil content of the
mash can be brought to 31% oil on dry fibre without nut breakage. If the pressure is
increased in order to reduce the oil content of the fibre to 20%, nut breakage increases
abruptly to 20% or even 30% .

There are two methods of modifying the composition of the digested mash with a
view to increasing the proportion of fibre:-

(i) Partial or total removal of the nuts

(ii) Addition of fibre to the fruit

Oil content of fibre and corresponding nut breakage

in relation to pressure (palm grove fruit)

23
 % Nut breakage

% Oil content in fibre

40

40
30
Volumetric equilibrium of nut & fibre

AH

30

BH 20

20

10

10

Pressure
0
“6” A “5” B “4”

Nut breakage Oil content in fibre

(i) Nut removal (de-pulping)

De-pulping is carried out in a knife de-pulper. The apparatus consists of two rotors
revolving at high speed in opposite directions. The gap between them is sufficiently
wide to enable pulp but not the nuts to go through.
The de-pulping of half of a batch of palm grove fruits increases the pulp content of the
digested mash from 40% to 57%. The proportion is similar to the composition T x T

24
fruit. When this mash is subjected to screw press extraction the residual oil content in
fibre can be brought down to 15% without causing any nut breakage. The
disadvantage of the process is that 50% of the nuts will have a very high oil content
requiring special treatment for its recovery.

De-pulping trials were carried out on fruits before and after digestion. From the point
of view of losses on nuts both processes are identical but the clogging up of the
machine is more pronounced with digested material. As an example, it may be
mentioned that the nuts removed in the mechanical de-pulping process never contain
less than 3% of oil. Since in the palm grove bunches the nuts represent 60% of the
fruit and the latter’s oil content is only 20%, the oil lost in nuts represents 10% of the
total oil.

An attempt has been made to wash the nuts with a view to recovering that oil. The
operation does not present serious difficulties. It was carried out with a powerful
centrifugal pump recycling water continuously. Unfortunately, the oil is emulsif ied
and separation must be carried out in a high speed centrifuge. The addition of a
washing installation and oil recovery station complicates the problem considerably.
The washing effect is more efficient with water containing a surfactant.

(ii) Addition of fibre

This was tried out on screw press having capacities ranging from 2 to 14 tonnes FFB
per hour. Undeniably, it makes it possible to reduce nut breakage and it improves the
extraction of the oil from the cake.. The results were better on small presses. Fibre
was added at the rate of a few percent to nearly 100% of the weight of fruits.

Such additions greatly reduce the capacity of the presses. It is difficult achieve
homogeneity of the mixture of the fruit and fibre, the handling of the large quantities
of the latter being far from easy.

On the average, the addition of 50%of fibre makes it possible to reduce the oil content
in the fibre to 10-12% and nut breakage to 2-5 %. With 20% of the fibre the residual
oil content is 15% on dry solids and 5% of the nuts are broken. In the latter case, if
pressure is reduced until nut breakage does not exceed 1%, the oil content of the fibre
is 20%. Finally, if the fibre addition amounts to only 10%, approximately 20% of oil
on dry matter is left in the fibre whilst nut breakage is 7.5%.

It has been observed that even with ratios of fibre to9 nuts or pericarp to nuts boosted
up largely beyond the equilibrium value, nut breakage still occurred. This is due to
lack of homogeneity of the nut and fibre mix and to the absolute size of the nuts.
Effectively, digestion leads to homogeneous mixture only if the addition of fibre into
the digester is carried out steadily ( 4-5 kg per addition). As regards the effect of the
absolute size of the nuts, there is a probability for some of the nuts to come into
contact with each other and with the cage at the outlet of the small press since the
cake thickness at that point is 50 mm. In large size presses the distances between the
screw and the cage is 90 mm. The cake is thicker and the chances of the nuts being
“squeezed” are less.

25
 5. MISCELLANEOUS
(i) Nut breakage

Generally, nut breakage is less important in a press yielding a thick cake. Broken nuts,
i.e. those which are no longer whole can be classified into split, chipped and crushed
nuts. The tearing of the shell occurs only with nuts with shell thickness of
approximately 1 mm. In that case kernels can be recovered. Their tegument is often
torn off and the albumen becomes apparent. It is sometimes possible to recover the
kernel from a chipped nut but generally the kernel is damaged. Crushed nuts of course
yield kernel dust.

Mention has been made elsewhere of the beneficial effect of high temperature of
nuts on breakage.

(ii) Perforated central shaft

Three of the presses under study possess in fact two perforated cages, an outer cage
and an inner one. The major part of the oil flows out through the outer cage. A small
amount (10 to 50 litres of pure oil per hour) flows through the inner cage.

On one of the presses with a capacity to process only one cage only it was observed
that the central part of the cake had higher oil content than the periphery. The addition
of an inner cage having 50 mm diameter readily improved the efficiency of oil
extraction from the cake.

In the course of the study of presses, it was observed that the cake had a lower oil
content immediately after the commissioning of the press than after a few hundred
hours of operation. This may be explained by the gradual wear of the press and the
cages and also by the increasingly greater ease with which the cake is expelled from
the cage. In other words, a pressure setting suitable for a new press may prove
inadequate after the press has been used for some time. To compensate for the wear
effect, the pressure exerted on the cake can be increased by suitable adjustment of the
pressure mechanism.

(iii) Ratio of the screw speed.

In the presses with coaxial twin screws, the speed ratio of the screws and
consequently that of the resulting volumes can be modified through suitable gear
selection. The effect of that ration was studied at Mongana on a small capacity press.
It is probable that the ratio must be selected according to the apparent density of the
material subjected to pressing ( fruits alone, fruits and trash, fruits and fibre, fibre
alone etc.). The density ranges from 1 in the case of fruit alone to 0.2 for fibre.

We give below the ratio of the gear s and the press speed for the press under test
(Bosondjo type) and that of the Yalingiba type presently delivered by the constructor.

26
 Bosondjo Yaligimba
Gear ratio 2.61/1 1.92/1
Speed ratio 1.7/1 1.24/1
Ratio of the resulting volume per hour (5 rpm) 16.6 m3 /6.3 m3 12.2 m3 / 6.3 m3

6. EXTRACTION BY NON-CONTINUOUS PRESS

This method of pressing was tried out in a revolving press capable of exerting a
pressure of about 97 bar (100 kg cm-2 ) on the cake. The cage had a height of I m and
a diameter of 0.520 m having a capacity of 212 litres.

A number of factors were examined, the most important ones being: number of plates,
pressure, duration of pressing, digestion, sterilization and the nut breakage. Contrary
to what has been done with the centrifugal and the screw presses in this case the study
will not deal with different type of fruits.

The Non-continuous press is actually more versatile and capable of dealing with
almost any type of fruit.

Number of plates

The number of plates does not seem to affect the oil extraction. No difference in the
oil content of the fibre was recorded when pressing was carried out without plates at
all or with an increasing number of plates until the cake thickness was reduced to a
mere 10mm to 20 mm. The only advantage in the use of plates appears to be the easier
unloading of the cake. When only two or three plates were used the discharge of the
cake was slow and laborious. The disadvantage of producing thin cake slices was the
increase in the percentage of nut breakage.

The utilization of partitions made of canvas was envisaged but according to the advice
of specialists no improvement could be expected there from. The object of canvas
partitions was to increase the porosity of the cake. Their use is fully justified in the
case of compact and closely packed cake (palm kernel cake etc.) but in the case of oil
palm fruit, the cake remains very porous even at the end of pressing owing to the
presence of fibre and nuts.

Partition Plates

The top and the bottom plates are thicker than the intermediate plates with the
diameter 9 mm smaller than the cage diameter. The plates may or may not be centred
but with d x p fruits if there is excess gap between the plate and the cage some press
cake may escape through the gap without being pressed. Even though the matter

27
ejected may be only a few hundred grammes it can trigger a significant pressure drop
(20% to 30%) in the press.

In addition to the adverse effect on the pressure the expelling of the matter can also
increase the dirt content of the crude oil. This sort of contamination occurs only with
dxp fruit.

The degree of oil extraction is contingent upon the intensity as the pressure build up
of the applied pressure but is not directly proportional to it. The effect decreases as the
pressure build up. For instance, the five results were recorded under standard
conditions shown in Table 1:

Table 1 .The pressure exerted on the cake and the oil loss

Pressure (kg cm-1 ) Oil on dry fibre (%)

30 33.3
60 23.2
90 22.4
150 20.7

The duration of pressing does not appear to affect the extent of oil extraction except in
the case of low pressure range.

Similarly, repeated pressure build-ups and releases are effective as long as maximum
pressure is not attained but two successive applications of maximum pressure do at
appear to have higher oil removal efficiency than one. In a totally enclosed press, it is
difficult to observe what happens but in Mongana, the flow of liquid through the cage
and into the crude oil receiving funnel was easily visible.

7. DIGESTION
Digestion had a marked effect on the efficiency of a non-continuous press, more than
that of centrifugal extraction. For instance two series of pressings involving 19 and 11
loads respectively were carried out. In the first, digestion was carried out at a shaft
speed of 17 rpm with eight beater arms. In the second the speed was 30 rpm with 10
beater arms fitted. The other conditions were identical (sterilization and pressing
cycle). The results are shown in Table 2.

Table 2. Effect of digestion on oil extraction efficiency

Oil on dry fibre Oil on nuts Settling coefficient

Insufficient digestion 26.4 1.5 0.975

Adequate digestion 12.2 0.7 0.984

28
Sterilization

Sterilization carried out with live steam at atmospheric pressure on D x P fruit

spikelets affects extraction efficiency. It can be observed that fibre feels greasy
between the fingers not only as a result of the high oil content( 30-40%) but also
because the pressure of a lot of cellular debris. It is opportune to recall that the above
conditions of sterilization an “oil wall” eventuate in the centrifugal extraction process.
Sterilization with flowing live steam appears to lead to “easier” extraction than
sterilization under pressure when operating on stored loose fruit.. “Easier” should be
taken to mean that application of pressure not up to maximum level leads to a higher
oil recovery. However, at maximum pressure the difference does not necessarily exist
any more. For instance, a 10 kg cm-2 pressure removes 80%of the oil contained in
fruits sterilized in live steam at atmospheric pressure against 50% for sterilization
done under pressure. However, after applications of a 75 kg cm-2 pressure, both cake s
are identical.

Triple peak sterilisation applied to bunch of any type pf planting material makes it
possible in the best conditions of digestion and at the rate of 6 pressings per hour to
record 11.5 to 14.0% oil on dry fibre and 0.5 to o.8% oil on nuts together with a
settling coefficient of 0.98. As has been pointed out else where, fibre with less than
10% oil on non-oily solids was obtained in a non-continuous press as a result of
eliminating an important portion of the cellular debris during digestion through the
use of a perforated bottom plate for instance. The cellular debris is thus drained off
into the crude oil and this lowers the coefficient.

In the case of fruit of high pericarp content the above mentioned rates of extraction
can be obtained practically without nut breakage. Serious breakage occurs when fruit
of low pulp content is extracted up to 12 to 14% oil on dry fibre.

Nut breakages were assessed in relation to applied pressure. Table 3 gives the daily
analytical results obtained on fibre and the percentage of broken nuts for five different
intensities of pressing. In order to set up the worst possible conditions, the fruit was
sterilised with live steam at atmospheric pressure for 20 minutes. Only steam jacket
heating was used during digestion (temperature of the mesh approximately 70 o C).
The shell did not therefore acquire springiness and kernels remained attached to the
shell. The nut breakage recorded must therefore be considered as maximum. It may
however occur at industrial scale in similar conditions of processing. The pressure
indicated in the table is that shown by the pressure gauge. The effective pressure on
the cake is approximately one third of it.

29
 Figure 1. Nut Breakage and Oil Content of Fibre in Relation to Pressure
24 32
% Nut Breakage % Oil on dry fibre

20 36

16 Zone of volumetric equilibrium 28

12 24

8 % nut breakage 20

0 16

4 12
50 100 150 200 250 300 Gauge Presssure
(17) (33) (50) (57) (84) (100) ( in kg / cm 2 )
Actual Pressure

Table 3. Effect of Pressure on Nut Breakage and Oil Content of Fibre

Pressure in bar (psig) % Broken Nuts Oil in dry fibre Moisture in wet fibre
49 (711) 1.0 35.8 53.1

98 ( 1450) 13.8 22.4 53.2

147 (2175) 21.5 20.2 52.0

196 (2900) 20.6 16.9 52.3

245 (3625) 19.9 14.4 47.4

294 (4350) 18.4 13.9 -

Figure 1 provides the pattern of residual oil in fibre and nut breakage. The diagram
should be compared with that of figure 2 obtained on a screw press. The observation
clearly lends support to the hypothesis of the equilibrium of fibre to nuts. It can be
observed that between 50 and 150 kg/cm2 (gauge pressure) nut breakage occurs. At
that point the void between the nuts is filled up and the equilibrium is attained. Nut
breakage ceases and the oil content of fibre follows an asymptotic curve.
As in the case of other two extraction processes in use (centrifuges and screw presses)
an attempt was made to press pericarp alone without nut specifically with the object
of evolving a procedure specially adapted to the fruit of palm groves. The results are
very similar to those recorded for the other processes: the pressing of straight pulp

30
leads to a lower rate of extraction than when nuts are present (17 to 18% oil on dry
fibre against 11.5 to 14% ). It can therefore be stated that, generally and regardless of
the process used, the extraction of straight pulp is not to be recommended.

Figure 2: Oil Content of Fibre and Corresponding Nut Breakage

in Relation to Pressure ( Palm Grove Fruit)

% Nut breakage

% Oil content in fibre

40

40
30
Volumetric equilibrium of nut & fibre

AH

30

BH 20

20

10

10

Pressure
0
“6” A “5” B “4”

Nut breakage Oil content in fibre

Post Pressing
After centrifugal extraction of the digested mash, the fibre contains from 13 to 25%
oil on dry matter and from 45 to 55% of moisture. The % of residual oil in fibre is still
too high amounting to 8 to 18% of the total oil. If the fibre is subjected to a pressure
of 50 bar the residual oil can be further brought down to 8-9%. The extracted crude
oil is very thick laden with solids. It contains approximately 20% of oil. Using

31
centrifugal separation only 80 to 85% of the oil can be separated due to the high solid
content. The balance oil remains attached to cellular debris.

(a) Post-pressing of fibre

The post-pressing of fibre was tried out in a vertical screw press in Mongana using a
pressure of even 300 bar-g. Fibre with oil content on dry matter ranging from 15 to
22% was tried out in the screw presses. After pressing in 2 tonnes/ hour press the oil
content pf the fibre was reduced to 8-11% on dry matter, higher than when pressing
fruits in the absence of nuts in the fibre. In practice post-pressing enables the recovery
of 2.5 to 4.5 % of the total oil, if a centrifugal process is used for the subsequent
separation of oil. Through static settling, that is by dilution, boiling and settling even
after repeating several times only one third of the oil was recoverable.

Generally , the handling of fibre is difficult. Extensive humidification is essential for

efficient oil extraction. Numerous difficulties were encountered in the passage of fibre
through the digester which incidentally was solely used for heating
The oil derived from pot-pressing was apparently identical to pulp oil from with
regard to oil quality (FFA, peroxide value, carotenoid, content and bleachability)
provided fresh fibre was used.

As it was observed that the pressing of the fibre was less effective than that of the
fruit, calyx leaves, intended to act as a filtering material , were added to the fibre. The
addition failed to improve recovery of oil.

Post-pressing undeniably permits to recover part of the oil left in the fibre.
Centrifugal separation of the crude oil is seen to give good extraction efficiency. The
handling of fibre entails certain amount of problems, which could be addressed by
using cyclone to feed the press and by heating the fibre through steam injection in the
press itself. The hourly throughput of the presses is greatly reduced when operating on
fibres (75% of the capacity of fruits)

(b) Simultaneous post-pressing of fruits and loose fruits

It has been well proven that the segregated processing of loose fruits led to a marked
improvement of the quality of the oil derived from bunches as regards FFA content as
well as bleach ability , stability etc.

Similarly , it has been mentioned that the recovery of oil from fibre by post-pressing
was possible but that the efficiency was lower in the absence of nuts. It was therefore
logical to combine processing of loose fruits with post-processing of fibre as a means
of introducing enough nuts to ensure efficient removal of oil from the fibre.

A series of tests were carried out with varying proportions of constituents within the
range 16/100 to 80/100 of fibre to fruit ratio. Beyond the latter ratio, digestion does
not take place normally and voids occur in the digester. Beyond a ratio of 80 to 100
fibre to fruit ratio, lumps also obstruct the digester outlet. Loose fibre at the outlet of
the cyclone has a density of 100 to 150 kg M-3 . This increases to 200-250 kg M-3
under the effect of light compacting. Fibre is sent into the digester with the latter
density. In the case of a larger excess of fibre over fruit ( 6 to 1 for instance),

32
digestion must be prolonged considerably, the degree of digestion being completely
inadequate after 40 minutes. Loose fruit processed together with fibre was of Dura
origin to the extent of 25 to 50%. The fibre used in the post processing was derived
from centrifugal extraction. Its oil content was 15 to 20 % on dry matter.

To determine the efficiency of the process it is necessary to assess separately the oil
derived from the fibre and from the fruit. To that end, the weights of the following
elements were recorded:- (a) Initial fibre (b) Fruit (c) Total crude oil (d) Total
clarified oil (e) Final fibre.

The oil content of the initial and final fibrewas also determined. From the data, it was
possible to allocate oil and to calculate the coefficients α β and γ . As only one
average β γ coefficient can be established for crude oil, the coefficient β may be
slightly over –estimated for the fibre and under estimated for the fruit.

Summing up, the coefficient α, for fibre ranged from 0.500 to 0.600 (depending on
the oil content of fibre) ; that of the fruit ranged from 0,950 to 0.965. The overall
efficiency of α β and γ varied from 0.450 to 0.560 for fibre and from 0,875 to 0.905
for the fruit. Contrary to expectations, the addition of fruit to fibre (or shell to fibre
for that matter) does not make it possible to attain the rate of extraction recorded with
a screw press. The post pressing of fruit and fibre yielded fibre with average oil
content of 10% on dry matter. This is twice as high as normal. The hope placed in that
process failed to materialize except for nut breakage

In the above process as well as the post pressing of fibre alone, the clarification of
crude oil was carried out by batch settling and by centrifugation. In one of the trials,
static separation was carried out repeatedly. The aqueous phase was drained off and
subjected to centrifugation instead of being discharged as in the conventional process.
The result of the test enables a comparative assessment to be made of the following
possibilities:

(a) Static separation (with 3 treatments)

(b) Single static separation with centrifugation of the aqueous phase.
(c) Centrifugal separation of crude oil

TABLE 1. EFFECT OF THE C;LARIFICATION PROCEDURE

ON THE RATIO OF LOST OIL TP TOTAL OIL

Static Static Separation Centrifugal

Separation & partial Separation of crude
centrifugation oil
Primary sludge 7.3% 7.3% 2.7%
Secondary sludge 3.2% 3.2% 1.7%
1st Interface 2.1% 0.5% 0.5%
2nd Interface 0.2% 0.2% 0.2%
3rd Interface 7.1% 0.9% 0.9%
Overall loss 19.9% 12.1% 6.0%
Oil recovered 80.1% 87.9% 94.0%
100.0% 100.0% 10.0%

33
The extraction process employing centrifuge and the press need large amounts of
mechanical power but the wet process uses water for the removal of oil. At first
(1922), the aim of the process was to separate completely the mesocarp of the fruit in
order to obtain clean nuts because at that time the separation of the cake produced by
the dry process into fibre and nuts was not well established.

Complete de-pulping by aqueous washing proved difficult. It could only be achieved

through prolonged digestion, as the fibre could not easily be washed away compared
to the cellular debris, which readily could be washed away from the digester. The wet
extraction process was therefore restricted to the recovery of the maximum amount of
oil within reasonable time.

The study of the standard wet process was resumed. The factors likely to lead to
maximum oil recovery were investigated. Moreover, the initial aim, that is complete
de-pulping was revived and it was envisaged to make the process a continuous
operation.
The wet extraction process therefore involves:

• The removal of oil by aqueous washing

• The separation of the oil from the wash water.

For a clear understanding of the washing process, it is logical first to examine the
retention of oil in the wash water.

Retention of oil in the Wash Water

The wash water consists of free oil, an emulsion of oil in water, cellular debris and
water containing a large amount of dissolved solids. The free oil and that in the
emulsion can be separated by static separation or if desired by centrifugation. The
cellular debris or the sludge contains a lot of oil. Only part of it can be separated by
settling. More oil can be separated under the effect of intense centrifugal forces but a
portion, which may be called the residual oil remains attached to the solids. Finally no
significant amount of oil is left in the water phase.

Through prolonged centrifugation of wash water in a tube, separation of the following

phases is obtained from top to the bottom: an oil layer, oil water inter- phase, and
solids deposit consisting of cellular debris. The interfacial layer contains cellular
agglomerates, that is whole intact cells generally lumped together.

Extraction of Oil from Cellular Debris.

Cellular debris have been subjected to a large number of treatments with a view to
freeing the oil attached to them. It is not possible to describe the hundreds of tests
carried out.

In principle, after the application of a specific treatment, the sludge was centrifuged.
The oil recovered and the residual oil in the cellular debris was determined. High
speed centrifugation (254,000 G) of sludge heated up to a high temperature was

34
proven to be no more effective than the ordinary laboratory centrifugation (3 to 6 000
rpm with a 25 to 40 cm diameter rotor).

The following treatments were applied:

• Drying and re-hydration

• Autoclaving, single or repeated with quick pressure release.
• Washing or turbo mixing with a variety of surfactants.
• Grinding
• Modification of the viscosity and density of the medium
• Modification of the pH.
• Effect of the dissolved salts. ( sodium chloride, ammonium sulphate, sodium
carbonate).
• Effect of alcohol (ethyl and methyl alcohol, glycerol)
• Saponification of the sludge
• Combination of two or more of the above treatments

Cellular debris shows a remarkable stability to these treatments as regards the oil
content, which invariably maintains itself at about 20% on dry basis.

Only solvent extraction carried out on partially or completely dry material makes it
possible to extract the oil from the cellular debris (Acetone does not require complete
desiccation prior to extraction).

Some of the treatments tried in the laboratory were applied at the industrial scale. The
results conform beyond doubt the consistency of oil retention in the sludge.

An apparent fact however became apparent. Whilst it is not possible to lower the oil
content of cellular debris below the 20% level, a non negligible portion of these debris
can however be solubilised. After dissolution in water, that fraction loses its retention
power. This mechanism will be examined in greater detail in chapter IV.

Therefore, waste water may contain less than 20% oil on total non-oil solids but as a
corollary, a portion of the NOS must be dissolved in water. After separation of the
soluble fraction, the oil content of the insoluble NOS will actually amount to 20%.
The insoluble NOS consist solely of cellular debris and no longer contains water
soluble protoplasmic matter.

Moreover, the fibre possesses a lower oil retention power than cellular debris because
of the lower surface to volume ratio. The insoluble matter of purely mineral origin
such as sand does not have any oil retention power.

Oil in cells.

Fresh oil cells or lipid cells contain 90% oil. The oil can flow out of them only under
certain conditions. Living cells have the property of retaining oil very strongly. Only a
small portion of it can be extracted in the fresh state by laceration, digestion,
centrifugation or pressing. Some factors induce a weakening of the cell membrane
and of the intercellular cement. They lead to oil exudation and dislocation of the cells.

35
The weakening of the cell membrane may consist in the permeation of tissues , which
are impervious when fresh and in the lowering of the mechanical resistance up to and
including rupture. The weakening of the membrane shows up in the flow of a flow of
virgin oil, whilst that of the cement (entailing break up) reveals itself by the
occurrences of lumps of cells or of sludge. Virgin oil in this context means the oil
exuding without intense grinding action exerted on the fruit

It has already been mentioned that the conditions required to induce the flow of virgin
oil during grinding or digestion of the fruit are as follows: Sterilization with live
steam at atmospheric pressure and the processing of old fruit. In this context, old fruit
means three days (or so) old loose fruit. In some instances the virgin oil so collected
contains only 2.6% of moisture and 0.4% of dirt. Sludge flows profusely in the
course of dry digestion of old loose fruit sterilized under high pressure. Neither of
these occurrences depends on the genetic origin of the fruit. Unfortunately, the flow
of the virgin oil does not permit to recover more than 30 to 40% of the total oil.
Extraction of the balance requires necessarily the loosening and the breaking up of the
fruit cells.

As has been correctly pointed out by Kehren it would be necessary to harden the
cellular cement to increase the chances of breaking up the cells in the course of
digestion and to avoid at all cost, the migration of unbroken cells into the crude oil.
The intercellular hardening can be achieved by addition of lime. The technique has
been tried: emulsions form and it is extremely difficult to break them up. It also
results in fibre with abnormally high oil content.

Another way of increasing the chances of breaking up the cells is to allow them the
leave the digester only after relatively long resident time. It has been observed that as
the sludge begins to flow, one out of every two or three cells emerged form the
digester without having shed the oil it contained. The extent of the potential oil losses
can be established by the determination of the oil bound to cellular debris emerging
form the digester in relation to the time of digestion. It can be observed in Table 1
involving eight tests that the retention of oil is less intense at the end of the digestion
process (The determination was carried out by repeated centrifuging and extraction of
solid deposit).

It is reiterated that. On the average, the cellular debris in the solids separated by
centrifuging contain50% of water soluble matter. Desiccation also induces hardening
of the intercellular cement. On the contrary, as has been mentioned previously, steam
under pressure breaks up the cement and leads to the formation of a large amount of
sludge.

36
TABLE.1: THE EFFECT OF DIGESTION TIME ON THE OIL LOSS TO CELLULAR
DEBRIS

OIL LOSS ON NON-OILY SOLIDS (NOS)

TRIAL
0 TO 10 10 TO 20 20 TO 30
MINUTES MINUTES MINUTES
1 54 12 12
2 28 12 17
3 22 12 11
4 38 22 11
5 58 22 12
6 63 17 11
7 39 20 18
8 28 23 21
AVERAGE 41.2 17.5 14.2

It appears therefore extremely difficult to break up all cells before they leave the
digester. It is also possible to envisage the break up of cells after they emerge form
the digester. The laboratory experiments showed the difficulty in the process.
Enzymatic treatments were applied to the cells and the cellular debris with a view to
facilitate the flow of oil. In some of these treatments pectolytic , amylclytic and
proteclytic enzymes were used. Mechanical treatments such as grinding with sand
have given slightly better results.

Recovery by Washing

The recovery of oil with water is carried out in the digester fitted with a perforated
bottom. Operating on loose fruit sterilized with live steam at atmospheric pressure,
with five to ten minutes digestion even at low speeds brings about a flow of virgin oil.
After that period of time the mesh is washed with a volume of hot water equal to 100
to 150% that of the fruit. At the end of the operation the digester will have only all
nuts and some fibre representing 5-20% of the total non-oily solids. In the
exceptional case of a digester fitted with numerous beater arms, it may be that only
traces of fibre are left in the digester after digestion and washing. The number of arms
affects greatly the residual quantity of fibre after digestion but has no influence on the
extraction of oil from the fibre. In the wet process, it is therefore an advantage to use
digesters fitted with a reduced number of arms.

The oil content of the fibre ranges from 8% to 15% on dry basis because of the almost
complete absence of cellular debris. As a consequence, the loss of oil on fibre left in
the digester amounts in practice only to approximately 1% of what was initially
present in the fruit.

With branches, which requires sterilization under pressure, provision for drainage
before washing is not necessary since no flow of virgin oil takes place. The extraction
of oil from bunches harvested in estates is more difficult because of the higher
proportion of pulp in addition to the trash accompanying the stripped fruit. The water
addition to wash away the solid particles temporarily makes the cake impervious
causing it to swell.

37
If the percentage of pulp exceeds 40%, the volume of wash water must be increased
beyond the 100 to 150% limit. For instance in the case of fruit with 60% pericarp,
twice as much water must be used. (This appears to be the highest practical limit) in
order to leave no more than 12 to 15% of oil on dry matter in the fibre.

Through prolonged washing, the oil content on non oily solids can be reduced to the
approximately 8-10% but the amount of oil taken up in the last few washings is
probably not recoverable. (the separation of oil from the wash water is discussed in
the next issue).

Among the other factors examined in the study of the wet process, the following may
be singled out:

FACTORS EFFECTS

1 FOR A GIVEN VOLUME OF The time taken to carry out the extraction does not
WASH WATER seem to affect either the residual oil content of the
fibre or the settling ability of the crude oil

2 EFFECT OF SURFACTANTS Surfactants do not appear to affect the efficiency

of the process except when used at high
concentration when they exert a detrimental effect

3 SUBSTITUTING SLUDGE Trials showed that only screens with large

CENTRIFUGE WITH perforations (12 to 20 mesh) allowed the wash
VIBRATING SCREEN
water to go thorough.

4 STATIC SEPARATION OF THE Whether wash water is diluted or not, the

WASH WATER efficiency of the operation does not exceed 75%
in the case of palm grove fruit and hardly reaches
55% with fruit containing a high proportion of
pulp

8. CONTINUOUS WET PROCESS

Counter-current washing with water in an inclined screw conveyor of digested fruit

did not give satisfying results.
A completely different method was tried but it needs further study. It consists in dry
grinding of the fruit and in receiving it in a tank full of boiling water The tank is
connected to a powerful centrifugal pump. The water is recycled after passage
through an apparatus, which separates the fibre and nuts. Part of the water laden with
oil and sediments is strained and treated in a continuous bowl centrifuge for
separation of the oil. A certain amount of wash water is recycled ; theoretically, the

38
efficiency of the process could reach 95%. The special feature of the process lies in
the relatively time consuming dry grinding and in the passage of the digested fruit in
the centrifugal pump.

In any event, it seems highly probable that a wet process can be evolved.

Extraction with Saturated Steam

The method is described by Kehran (lee.cit.) and is patented. It was tried in Maongana.
Undoubtedly, saturated steam make it possible to extract 40 to 70% of the oil
contained in the fruit without powerful mechanical means and without addition of
water but only on old loose fruit sterilized with live steam at atmospheric pressure.

Owing to the fact that crop processed in the form of old loose fruit represents only a
small proportion of the total Congo production, the method is of very limited interest.
The results of three extraction runs with saturated steam are given below:

TABLE. 3. THREE METHODS OF OIL EXTRACTION

Percentage of Extracted oil

Treatment
Old detached fruit from palm D xP fruit sterilized under pressure
grove sterilized with live steam Fresh 48 hours old
After treatment with 63.0% 0.0 % 21.0 %
saturated steam
After washing 28.6 % Traces Traces

After Dry digestion 1.9 % traces 34.7 %

After digestion and 4.9 % About 98 % About 43 %

washing

Solvent Extraction

The method does not seem to be a profitable proposition in central Africa in present
circumstances. It might become financially attractive for the recovery of oil from
some of the waste products of processing. The extraction with a number of
solvents( benzene, hexane, tolene, ethyl alcohol) were studied particularly with a view
to evolving a method for the determination of the oil content of large quantities of
material or waste products, also for the extraction of carotanoids from fibre (IRHO
Principle).

Comparison of the various extraction Processes

1. Wet extraction process

The method requires centrifugal separation as static separation gives rise to

extremely high losses. Wet extraction followed by centrifugal separation is used at
present solely on old loose fruit, in practice, only the fruit from palm groves.

39
Attempts to substitute strainers to sludge centrifuges have been unsuccessful. In the
case of plantation crop in the form of bunches sterilized under pressure, the efficiency
of oil extraction cannot reasonably be expected to exceed 90% even on the
sssumption that a solution could be found to the problem of straining and on the
understanding that the filtered wash water would be subjected to high speed
centrifugation. The processing of palm grove bunches gives results similar to those
recorded for the processing of T xT bunches.
The procedure of extraction with saturated steam was tried as an off shoot of the wet
process. It enables recovery without powerful means of 40 to 70% of oil. Howver, it
can only be applied to old loose fruit sterilized with live steam at atmospheric
pressure. Its interest therefore limited.

2. Continuous dry grinding and wet process

This has an advantage of being able to apply to any type of fruit.. The process would
therefore compete directly with continuous screw press extraction since it would
permit almost complete automation

3. Extraction by centrifuges

The advantage of the process is to yield oil containing very little impurities. It can be
clarified easily by static separation but extraction efficiency appears to be limited to
90%

Test results show that oil losses in cake derived from palm grove old loose fruit are
very high. The reason is inherent in the very composition of the fruit. Pulp is
subjected to the pressure of nuts only at the beginning of centrifugation, so long as
there is volumetric excess of pericarp over nuts.

It5 should be noted that the processing of palm grove bunches always leads to less
satisfactory results than the processing of manually detached loose fruits because of
the additional loss incurred in the bunch refuse and also because of the increased non-
oily solids content of the fruit. These solids absorb a large amount of oil. During
investigational work on centrifugal extraction, the following observations were
made:-

• The centrifugation of thin layers of material which was studied with a

view to evolving a continuous centrifugal extraction does not seem to
provide good extraction efficiency.

• D X P fruit sterilized under standard conditions induces the formation of

an oil wall in the centrifuge. The wall can be prevented from building up
through a series of appropriate steps, notably the addition of nuts.

• Slow acceleration (100 minute-2 ) does not improve extraction.

• The centrifugation of pericarp alone without nuts leads to lower extraction.

40
4. Extraction by discontinuous press

The cake obtained through that process has a lower oil content than that from
centrifuges. The crude oil is however, less pure than its ability to settle is not as good.
As a result the efficiency of presses is not markedly higher than that of centrifuges.

Presses are more expensive than centrifuges and maintenance is more difficult

5. Extraction by Continuous press

The continuous pressing of palm grove fruit can not be considered with the
equipment tried at Mongana owing to nut breakage and poor extraction of oil from
the cake. It is however, possible to process that kind of fruit in a continuous press
either by partial or total removal of nuts from fruits or by adding fibre to the digested
mash.
Removal of nuts appear a satisfactory solution because of thjr necessity of washing
them and, moreover, because the separation of oil from the wash water implies the
use of high speed centrifugation.

On crop containing low proportion of Dura material, the extraction efficiency of the
continuous press is markedly higher than that of other processes.

Very little labour is required to operate it. Minimum floor space is needed for its
installation. In terms of cots per tone of FFB processed its cost is lower than that of
the discontinuous presses or centrifuges. The cake can be dealt with more easily
because of the low content in oil, moisture and cellular debris. The power
consumption per tone of FFB is low and without peaks. The disadvantages of the
continuous press compared to other processes are:

• The crude oil must be necessarily screened and centrifuged.

• The press is of more sophisticated conception than the centrifuge. The risks
of breakdown are greater and so are spare parts requirements. However, from
that point of view the continuous press compares favourably with
discontinuous one.
• Nut breakage reaches 5-10% with T x T material and 0- 2% with D x P.

9. CLARIFICATION OF CRUDE OIL

General
Whatever the process used, crude oil must be refined. The complete refining of oil
consists of the following operations:
➢ separation of solid impurities that is impurities not soluble in oil;
➢ separation of free water;
➢ partial separation of dissolved moisture that is dehydration or drying;

41
 ➢ de-gumming;
➢ separation of free fatty acids or neutralization;
➢ separation, reduction or destruction of pigments, that is bleaching; and
➢ separation, reduction of destruction of volatile compounds affecting odour or
taste that is deodorization.
Neutralisation, bleaching and deodorization are really part of the refining
process and are generally carried out by the user of oil and not by the producer. They
were therefore not studied.

Separation of Solid Impurities

The separation is often carried out simultaneously with that of water. It can be
achieved by:
• settling;
• screening;
• centrifugation; and
• filtering.
Settling
The speed of sedimentation is governed by the Stokes law, which is applicable to
particles of any dimension except those of colloidal dimension.

The law is as under:

V = g D 2 (d 2 – d 1 )
18  Where,
V = speed of sedimentation
g = acceleration of gravity (981 cm/sec2 )
D = diameter of the particles
d 1, d 2 = densities of the two media
 = viscosity of the medium
The equation shows that the final speed is directly proportional to the square
of the particles diameter, to the difference in density of the particles and that of the

42
 medium and inversely proportional to the viscosity of the medium with all units
expressed in the c.g.s system.
The largest solid impurities to be separated are the fibre. The cellular debris is
the smallest. The length of the cell ranges from 20 to 100 microns. The width is
approximately 20 microns. Calcium oxalate crystals are approximately 100 microns
long often grouped into bundles of a large number of needles.
The viscosity of oil is shown in the graph of figure 31.
Centipoises
32

28
C.Poise
24

20

16

12

50 60 70 80 90 150 200 250

Temperature o Celcius

Figure 31: Effect of Crude Oil Temperature on Viscosity

The density of fibre and cellular debris is equal or higher than 1 and
sometimes is as high as 1.4. The diameter of the particles ranges from a few microns
to several millimeters. The approximate density of oil is given in Table 50 (vide
details in appendix).

43
 TABLE 50. APPROXIMATE DENSITY OF
OIL AGAINST TEMPERATURE

Temperature (°C) Density

20 0.925 – 0.935
30 0.910 – 0.920
40 0.900
50 0.890
60 0.883
70 0.876
80 0.869
90 0.863
100 0.857

The equation shows that, all other conditions being equal, the settling rate at
100°C is twice as high as that at 70°C and 3.5 as high as that at 50°C.
For 20 microns particles, the equation gives a settling time of 5 hours for a
distance of 1 meter and a temperature of 80°C. The speed of sedimentation is slowed
down by convection currents in the settling tanks. These currents can be minimized
by the lagging of the tanks.
The proportion of water and impurities in crude oil derived from the various
extraction processes is extremely variable as shown in Table 51.

TABLE 51. COMPOSITION OF CRUDE OIL

Extraction % Oil % Water % NOS Rate of settling
process Range Average Range Average Range Average in arbitrary
nuts
Centrifuge 70 – 90 80 10 – 25 17 1–4 3 8.5
Press 65 – 90 75 10 – 30 20 3–6 5 7.5
Screw press 40 – 75 66 10 – 40 24 6 – 25 10 0.5
Wet extraction 10 – 25 16 70 – 85 - 3–7 - 2.0

By measuring in identical containers the height of oil separated in relation to

the total amount of oil, the relative settling rate was determined; the results are given

44
in the last column of Table 51. The procedure is not very accurate. Moreover, in the
case of crude oil from continuous presses a number of factors affect the rate of
settling, particularly screening ,which improves separation, boiling, dilution etc.
This question has been studied in detail.

Settling of screw press crude oil

Is should be stated again that in the continuous pressing process, approximately ¾ of
the pericarp find their way into the crude oil. In other words, the production of 1
tonne of clean oil by that process implies the removal of oil from approximately 150
kg of dry solids derived from the crude oil (30 to 40 kg in the case of oil from the
centrifugal extraction process).

Dilution of crude oil

Dilution of crude oil greatly affects settling. The study of the settling of press crude
oil in relation to dilution shows that the rate of separation is highest for the undiluted
crude oil that it slows down for a 50% dilution then increases again if dilution is
further increased. From that point the rate of settling appears to remain constant.
A close relationship seems to exist between the viscosity of crude oil and rate
of settling. The variations in the viscosity of crude oil and plotted in figure 32.

Viscosity

Rate of settling

Ml/min

0 50 100 150 200

Dilution %
Figure 32: Dilution Rate and Rate of Separation of Crude Oil

45
 What explanation can be found for the marked variations (increase
then decrease) in crude oil viscosity as a result of water addition? The
centrifuging of press crude oil in a laboratory centrifuge gives some insight
into the problem.

After a sufficiently long time of centrifugation a supernatant layer of

clarified oil and a plug of sediments can be observed. If the same treatment is
applied to the crude oil from centrifuges three components and not two as
before can be seen. A third one, water occupies a portion of the tube between
the oil and the sediments. It may be concluded there from that in the crude oil
from centrifuges there is an excess of water over that of the saturated
sediments, whereas in the case of press crude oil, the sediments are at the most
saturated without excess of water.

Referring to the data of Table 51, It can be noted that the ratio of NOS
to the water in centrifuge and press crude oil is 3 to 17 and 10 to 24 or 25
respectively that is 1/5.6 and 1/2.4. The ratio of water to sediments is
therefore higher for centrifuge crude oil.
In order to increase that ratio in the press crude oil let us add 10, 20,
100 and 200% of water for instance. The centrifugation of the diluted samples
shows that when dilution reaches 50%, that is when 50 parts of water have
been added to 100 parts of crude oil, a middle layer of water starts forming
between the supernatant oil and the sediments. At that point, the sediments
are saturated with water containing 5 times (centrifuge) and 7 times (press)
their weight of water.

At the beginning of dilution, the sediments absorb water (increase

in viscosity and decrease in rate of settling). When they are saturated the
rate of settling increases (increase in density, decrease in the viscosity of
the sediments and of the medium).

It has been further observed that in the case of dilution close to

saturation, the viscosity continues to increase up to certain limit in the course

46
of heating. It may be inferred therefrom that water absorption or swelling is
probably not an instantaneous reaction.

It may be added at this stage that sterilized fruit (dry or wet) also
absorb water under the pressure existing in the digester. At Mongana,
contrary to some assertions, the addition of water into the digester (up to
150 kg of water per tone of fruit) has never been observed to induce a
flow of sludge.

The dilution of crude oil appears to decrease the stability of the

suspension of impurities in the oil-water mixture. In the case of static
separation, the aim is to speed up sedimentation but for the centrifugation of
crude oil it is advantageous to maintain the maximum amounts of solids in
suspension (vide experiments on increasing stability through addition of
carboxy-methylcellulose).

The fact that extensive dilution of crude oil decrease the stability of the
suspension can be explained by changes in superficial (or inter-facial) tension
and by the exchange of electric charges with the water contained in the fruit.
The latter water is highly laden with protective colloids.

As stated in the preceding chapter, static separation of press crude oil

does not lead to satisfactory recovery of oil from the sludge. The process
could not therefore be used industrially. However, it is probably possible to
recover a large amount of oil from the settled crude oil and then centrifuge the
sludge.

A diagram of static separation of boiled undiluted press crude oil in a

200 litre vertical tank made of plexiglass is given below:

47
 % Settling of oil
on total crude oil

0 10 20 30 40 50 60 70 80
Time in minutes
Figure 33. Static Dilution of Undiluted Press Crude Oil

TABLE 52. STATIC SEPARATION OF UNDILUTED PRESS CURDE OIL

Time % Oil Differential

5 13 13
10 21 8
15 25 4
20 28 3
25 31 3
30 33 2
40 35 2
60 35 0
80 35.4 0.4

The figures show that after 40 minutes almost all the oil that can be
separated has come up to the surface. At the point, there remains 65% of
homogeneous sludge. After dilution of that sludge with an equal volume of
water and a period of rest of 12 hours, oil to the extent of 2.5% of the initial
amount is recoverable at the surface. The secondary sludge contains the
following:
• 16.5% oil in the top portion;
• 9.0% oil in the middle portion; and
• 8.0% oil in the bottom portion.

48
 A further period of settling does not lead to the recovery of additional
oil. Further dilution has practically no effect. This confirms the statement
made previously. Approximately 70% to 75% of the oil settles quite easily but
the balance of 25% cannot be separated by dilution and static settling.

The static separation of screw press crude oil does not present much
practical interest. By contrast, continuous settling possesses numerous
advantages. For this reason it was tried industrially as an experiment and was
studied in the pilot plant. In the trial at industrial scale, the crude oil subjected
to settling was a mixture derived from a continuous press of 14 tons bunch per
hour capacity and centrifuges (Bosondjo).
The separation of crude oil was carried out in a 5m3 settling tank. The
crude oil was produced by the press working at 67% of its capacity and from 2
to 4 basket centrifuges of 1.2 metre diameter. Settling proceeds at normal rate
for about 4 hours. At that point, sediments find their way into the decanted oil.
It is thus necessary to stop the crude feed for about 4 hours approximately.
That installation operated for several weeks. It made it possible to establish
the following. A settling tank of 5m3 is not sufficient to separated effectively
the crude oil output of a 12 to 14 tons capacity press. The tank volume must
be at least doubled. The oil layer in the settling tank (adjustable by the height
of the skimmer) must be thicker than that selected for the decantation of
centrifuge crude oil. It is not important to remove the sludge but the
separated oil should not contain more than traces of impurities. The sludge
containing approximately 10% of oil and 5% of non oily solids does not settle
further. Finally the NOS content of sludge is virtually the same for the top and
the bottom portions.
This last observation indicates that the removal of sand from Colin
press crude oil diluted with an equal volume of water is not possible by static
settling.

In the pilot plant, clarification was carried out in a continuous settling tank of
220 litres capacity Figure 1. The conclusions drawn from experiments carried
out are summarized below:

49
Capacity The 220 litres settling tank has a working volume of 150 litres. It can
cope with 500 kg of diluted crude oil per hour (100% dilution with
water). Crude oil therefore settles for approximately 18 minutes

Oil recovery Approximately 60% of the oil is recovered

Separation Almost total separation is achieved since only 1.5% of the impurities
of NOS find their way into the oil. The average moisture and dirt content of the
continuously settled oil is 1.3% and 0.06% and would not be suitable
in an industrial process.

Interface At times the interfacial layer tends to increase and occupy the space
intended for clean oil (density close to that of oil). At that point, the
crude oil feed is reduced slightly and after a few minutes, enough oil
has separated to enable continuous settling to take place again. The
hourly capacity of 500 kg allows for the slowing down of the feed.

Removal of The output is steady. The composition of sludge is constant. Oil

sludge content ranges from 11 to 13% and NOS from 4 to 6.5% (12 analyses)

(b) Clarification of wet process crude oil

A lot of difficulties was experienced, probably as a result of the high colloid

content of crude oil. The efficiency does not exceed 65% to 70%.

(c) Clarification of centrifuge crude oil

The process offers no difficulties. A single static separation leads to an

efficiency of 94% to 95%. This may be increased to the 96.5% to 97.5% level
by second separation. There seems to be no advantage in carrying out
further separation.
The very fast settling of centrifuge or discontinuous press crude oil is a
consequence of the low content in dirt, colloids and other solids in suspension.
Among the latter, fruit pectins deserve special attention.

50
 Crude oil feed

Flexi -
Adjustable
glass
Level

Sludge

OIL

Sampling
Cocks

Live
Steam

Steam
Heating
Coil

Figure 1. Experimental Continuous Settling Tank.

It was pointed out in chapter III that the addition of surfactants was
tried in an attempt to improve the efficiency of oil extraction from the cake.
The addition was carried out either directly in the digester or by washing the
cake at the end of centrifugal run. It is of interest to mention the effect of the

51
 addition of surfactants on the settling characteristics of crude oil. For instance,
the rate of settling of three samples of oil is given graphically in Figure 1 (1)
control oil (2) oil treated with 0.025% of alkyl-aryl-sulphonate (3) Oil treated
with 0.5% of A.A.S.

The examination of graph in Figure 1 leads to the following observations:-

• the control oil separated completely after 30 min;

• no 2 oil separated completely after 13 min;

• no 3 oil decanted completely in 160 min. IN that experiment it was not

possible to boil the oil (this was done for the other two test) as a result
of the formation of a large amount of form (the tank overflow);

• the addition of water containing 0.025% of alky-aryl-sulphonate slows

down settling at the beginning of the operation, but the rate of settling
at the end of it decreases less markedly than in the case of the control
oil. As a result, the last 10% of oil of the control require 24 min to
settle whilst in the case of no. 2 oil only 5.5 min are needed; and

• the addition of 0.5% of alkyl-aryl-sulphonate slow down settling

considerably.

The analysis of the bottom layer in the case of oils No. 1 and 2 indicates that
after the time given above there is no more oil capable of further settling.

The same process was used with crude oil from continuous presses. No
increase in the rate of settling was recorded whilst quite a lot of oil was found to
remain in the bottom layer.

52
 5 Min 30 Sec LAST 10% OF OIL 30 MINUTES

100
% SETTLED OIL EFFECT OF SURFACTANTS
LAST 10% OF OIL 13 MINUTES ON THE RATE OF
SETTLING OF CRUDE OIL

75 7 MINUTES 30 SEC

WASHING AT
0.025% A.A.S

(1)
50
100% AT 160
Minutes
(2)

25
WASHING 0.5% A.A.S

(3)

5 10 15 20 25 30 Min

d) Factor affecting settling

It had been observed that screening improved the settling characteristics of

crude oil because of the coalescence of globules. A laboratory experiment
showed that subjecting crude oil to high frequency vibrations led to increased
settling ability. The technique was tried at semi industrial scale with screw
press crude oil subjected to ultrasounds. The apparatus consists of a bell with
a reed in its centre. The reed vibrates as a result of the flow of oil under high
pressure (frequency of 18 000 to 22 000 cycles per second).

Ultrasounds of that frequency do not induce coalescence of oil

globules. On the contrary, they greatly stabilise the emulsion. The use of
vibrating reeds connected to an electromagnet (frequency 50 c/s) leads to
coalescence around the reeds but no increase in the rate of settling is recorded.

As has been already mentioned, boiling improves the settling of crude

oil. If steam injection is used it should be ensured that the crude oil actually

53
 boils, and is not simply churned up by the steam. Some emulsions break only
at boiling temperature. They remain stable up to 90°C.
The dehydration of crude oil, if carried out far enough, enables fast
separation of the non oily solids. These can be removed. They contain 60%
of oil and can be pressed. Although dehydration of crude oil can be easily
carried out in the laboratory by the evaporation under vacuum it is difficult to
envisage a practical application of that technique. The fact that dehydration
makes good separation possible should however be recorded.
Similarly, the good settling characteristics of crude oil derived from
dehydrated fruit is worthy of mention (see annex 1).

Screening
Screening which has been applied on the oil derived from the four extraction
processes and on all types of fruit appears to be indispensable in palm oil milling. It
can be carried out on crude oil as well as on sludge after the first separation. The
advantages and is-advantages of the two systems were compared.
In practice, it may be concluded that the point of the circuit where the screen is
incorporated is not important. In all cases, the solids retained by the screen contains
a lot of oil and must be recycled.

Washing of the solids

The recycling of the solids is not a complicated operation but nevertheless requires
labour or power and entails additional expenditure, unless the solids can be
reintroduced into the digester by gravity. In order to do away with recycling,
7washing with water was tried either after the solids have been separated or whilst
they accumulate on the screen. The latter technique is preferable from the point of
view of oil recovery but it dilutes the crude oil and this is sometimes undesirable.
As an example, the composition of the solids is given in Table 1. They were
obtained from screening wet process crude oil through a 20 mesh strainer vibrating at
3000 rpm.

54
 TABLE 1. COMPSOTION OF THE SOLIDS RETAINED ON THE VIBRATING SCREEN

Unwashed solids (%) Washed solids (%)

Water of solids 74.0 82.3

Oil on solids 16.6 6.7
9.4 10.4
176.3 64.4

The solids were washed with a volume of water equal to that of crude oil.
The washing with wetting agents or amionic or anionic surfactants does
decrease the residual oil content. The content of the non oily solids is always very
high regardless of the origin of the screened material. It appears therefore
indispensable to recycle.
The following factors were examined in the study of vibrating screens:-
• frequency: 1400 and 3000 cycles per second. Improve results are
obtained through an increase in frequency;
• temperature: As a result of its effect on the viscosity of oil, temperature
markedly affects the efficiency of screening. The best results are
obtained at 100°C. Crude oil should not be screened at a temperature
lower than 50°C to 90°C; and
• size of perforations: Crude oil from wet extraction processes can be
screened on 20 mesh or coarser strainers. Hot undiluted press crude
oil passes through 20 to 30 mesh strainers. A second screening through
60mesh strainer for instance yields a large amount of solids constituted
mainly by cellular debris. Sequential double screening does not
appear desirable since the object of screen of screening is to retain the
fibre, which is a hindrance to centrifugation and not the cellular debris
from which oil is best recovered by centrifugation or even static
separation. Heated up crude oil from presses or centrifuges can be
easily screened, even on 120 mesh strainers. A large amount of solids
is however retained. 60 mesh strainers appear best suited.*

55
 TABLE 2: SPECIFICATION OF STRAINERS*

No. Size of perforation (mm) Diameter of wire (mm) Perforated area (%)
10 2.08 0.70 56
16 1.24 0.50 51
20 0.99 0.40 51
25 0.76 0.35 47
30 0.63 0.30 46
35 0.51 0.28 42
40 0.45 0.24 43
50 0.36 0.20 41
60 0.28 0.18 37
70 0.24 0.16 36
80 0.21 0.14 36
90 0.189 0.12 38
220 0.168 0.11 37
220 0.153 0.10 37
230 0.141 0.09 37
230 0.124 0.09 35
250 0.105 0.08 32
( French norms and number of strand per inch):

• feed: In order to used the whole of the screening surface, it is assential

to install a suitable distributor, possible of the flap type but a
distribution trough must also be fitted.
The above conclusion applies to standard vibrating screens used in oil
mills. The straining material is attached to a horizontal shaft eccentric.
Vibrations therefore take place in a vertical plane. The pattern of the
vibrations is governed not only by the type of screen but also by the distance
from the vibration making device. The shape of the vibrations can range from
a circle to a very elongated ellipse.
Another type of screening used in flour mills has been tried: The
“plan-sifter”. The vibrations occur in a horizontal plane, the shaft of the
eccentric being vertical. The screen has given excellent results, better perhaps
than the standard vibrating screens. The hourly capacity per unit is higher ,
whilst oil removal from the retained solids appears very effective. Additional
trials are in progress. The cost of these suspended “plan-sifters” is, for a given
output, lower than that of vibrating screen mounted on a frame.

56
Centrifugal screening
As a result of the difficulties encountered in the separation of the solids from
wet process crude oil, the filtration in a 1.20 metre centrifuge spinning at 1000 rpm
was tried with the whole surface of the basket lined with canvas cloth. Screening is
easy and the throughput very high.

The capacity of a standard centrifuge is sufficient to screen approximately six

tonnes of crude oil. The cleaning of the cloth is difficulty and time consuming. It is
contemplated to use shortly metal gauze with oblong perforations 0.1 to 0.2
millimeter wide and 4 to 5 mm long. The oil content of the solids is fairly low but
washing with water does not lower it further to a marked extent. Table 3 gives the
results obtained on wet process crude oil.
TABLE 3.
Solids retained on the screen (%) Washed solids (%)

79.3 73.6
Water on solids
5.1 6.2
Oil on solids
15.6 20.2
NOS on solids
32.6 30.7
Oil on dry
basis

Before closing this paragraph on screening is should be pointed out that

laboratory experiments were carried out on filtration of wet process and continuous
press crude oil with a view to studying the possible use of an industrial vacuum rotary
filter. The attempt was unsuccessful owing to the fast clogging of the filtering cloth.

Centrifugation
The problem of centrifugation may be approached in a number of different ways.
Some years ago, centrifugation was simply a purification process applied to oil
derived from primary and secondary static separation (expect in the case of the wet
process). Soon afterwards, at the time of the introduction of continuous settling,
purification of oil continued to be carried out by centrifugation but in addition, the

57
sludge derived from the continuous settling tank was also subjected to centrifugation.
That technique is now standard procedure for oil mill of average to large capacity.
Investigations were carried out with a view to eliminating completely the
separation of oil by batch or continuous settling and to replacing it by direct
centrifugation of crude oil. In the latter case two centrifugations are required, one of
these replacing the static decantation.
The following will therefore be examined separately:
• centrifugal separation of sludge; and
• purification of oil.

Centrifugal separation of sludge

At this stage it should be mentioned that if settling is not made use of, the centrifugal
separation of sludge becomes a requisite. This is because it is not possible to treat
crude oil directly in a purifier even when it is relatively pure like that derived from
centrifugal extractor. Bowls clog so quickly that frequent cleaning become necessary.
Their capacity is at the most 30kg of wet solids (for large centrifuges) corresponding
approximately to 6 kg of dry material. Even with crude oil containing no more than
1% of non oily solids, the capacity of a large bowl centrifuge (generally 12 kg of wet
solids, that is 2.5 kg of dry material) between consecutive cleanings would only be
600 kg if the whole of the NOS were retained in the bowl. This is of course not the
case. If it is assumed that 80% of the NOS find their way into the discharge the
capacity of the machine would be 3 tons of crude oil.
Before centrifugal separator of sludge the screening of undiluted or diluted
crude oil was found to be necessary. Even relatively clean crude oil contains a certain
amount of fibrous strands of length ranging from a few to 50 millimeters. In the
course of centrifugation, these strands accumulate at various places in the machine,
more particularly around the distribution holes of the plates and, eventually, obstruct
them completely. This fibre is not discharged from self cleaning centrifuges.
Eventually the bowl may go out of balance as a result. Screening is therefore
indispensable but there is no advantage in using too fine a strainer, which retains an
important portion of the cellular debris as centrifugation removes more oil from the
latter than screening. In this respect it is worth mentioning that it is an erroneous

58
concept to assess the effectiveness of a strainer solely by the amount of solids it
retains.
Generally, the sludge separating centrifuges discharge the aqueous phase from
crude oil continuously and may discharge solids either continuously or intermittently.
The discharged aqueous phase contains between 70 and 90% of the non oily solids of
crude oil. Half of the solids are dissolved and the rest is in suspension.
Three sludge separating centrifuges were studied at Mongana:
• Titan centrifuge – bowl with plates – intermittent and automatic
discharge of solids;
• Werkspoor centrifuge – bowl with plates – continuous discharge of
sediments; and
• Stork centrifuge – bowl without plates – continuous discharge of
sediments.
The capacity of the above centrifuges ranges from 2.5 to 12 tonnes per hour
according to the type of machine and the composition of crude oil.

Titan centrifuge
The frequency of bowl discharging is contingent upon the NOS content of crude oil
and more particularly upon the amount of sediments carried away in the aqueous
phase. That amount is directly related to the ability of crude oil to retain suspended
solids. Fibre and large lumps of cellular debris do not remain in suspension when
subjected to powerful centrifugal force. In the case of cellular debris of small
dimension, there seems to be an optimum concentration to keep them in suspension.
In order to increase the proportion of NOS removable by the aqueous phase,
the following procedures were tried:
• Increasing the proportion of soluble NOS;
• Increasing the viscosity of the aqueous phase discharge; and
• Removal of a portion of the sediments at the periphery of the bowl.
A larger proportion of the sediments can be solubilised by boiling the crude oil.
This question is discussed in another section. The increase in viscosity of crude oil
can easily be achieved in the laboratory by addition of CMC (carboxy-methyl-
cellulose), but at industrial scale the process was found to be ineffective. At the rate
of 1% and at 100°C, CMC exerts a marked effect but the cost is very high. A

59
concentration of 0.1% CMC still significantly modifies the viscosity but is too low to
prevent the separation of sediments under the effect of a large centrifugal force.
The continuous removal of a portion of the sediments can be achieved by a
series of nozzles fitted at the bowl periphery. The process is not very effective and
the capacity of the machine is reduced.
Based on results from tests carried out with that centrifuge difficulties can be
forecast when using it for crude oil having a high sand content. When the sediments
are forcefully expelled from the bowl at the time of the discharge, a marked abrasive
action occurs.
The use of that machine is justified for liquids with low impurities content
when the sediments can be discharged infrequently. Moreover, through a simple
change of the bowl plates, the machine can be converted into a purifier. Because of
the automatic cleaning, the converted machine possesses a marked advantage over
other types of bowl centrifuge in which sediments accumulate in the bowl. The
quality of the oil treated in that type of machine is quite comparable to that of oil
treated in conventional purifiers.

particles is the active agent. Approximately 0.5-3% of the total amount of material fed
into the reactor will be the catalyst. Reaction in hot oil of the synthetic production of
diesel from waste in 3 minutes reaction time in a high speed turbulence system.

The hydrated lime needed for the neutralization of dangerous by-products is to be

used only with chloro-fluoro materials, particularly with respect to PVC and PCB oils.
Neither the catalyst nor neutralizer are chemically dangerous and can be handled
easily, if carefully.

10. PROBLEMS ASSOCIATED WITH OIL SEPARATION

Werkspoor Centrifuge with Continuous Discharge of Sediments

The bowl is a star-shaped, 6 spokes rotor. A nozzle is fitted at the end of each of the
branches. A constant volume of water is (5.4 t hr-1 ) discharged through the nozzles.
The level of the interface is not set by gravity discs but by two inverted centrifugal
pumps (fixed rotor and rotating liquid). One of these pumps supplies enough water
to ensure full discharge of liquid through the nozzles the diameter of which could vary
from (2 to 2.3 mm.

60
 This machine has been used for various types of crude oil pumping especially
the crude oil discharged by the screw press. The limiting factor as regards to capacity
is the amount of aqueous phase to be separated from the crude oil and not the quantity
of oil. With a constant discharge of 5.4 t hr-1 of water, it has been possible to collect
up to 7 t of oil per hour. The main advantage of the machine is its ability to deal with
crude oil containing from 0 to 100% of oil without performing any adjustment in its
settings. Among the factors affecting the efficiency of the machine, the following are
worth noting.

• Hourly Throughput
Contrary to what may be believed, the efficiency of oil removal from the crude oil is
directly proportional to the hourly output and therefore inversely proportional to the
dwelling time in the machine. The analytical results versus the crude oil hourly
output are shown in the Table 1 below:-

TABLE 1. EFFECT OF TRHOUGHPUT ON THE OIL CONTENT OF NOS

Less then 2.5 2.5 to 4.5 tonnes More than 4.5
tonnes per hour per hours tonnes per hour

Oil on NOS 23.8% 19.9% 18.9%

percentage of 15% 28% 38%

results lower than
15%
53 54 45
Number of samples

It is difficult to give a satisfactory explanation to the fact, why a longer

dwelling time of the crude oil in the bowl should lead to a reduction in the extraction
of oil from the NOS. A logical explanation could be that during periods of low
hourly inputs , a larger volume of make up water is admitted into the machine to
maintain its stipulated throughput. As a result, the larger intake of water might create
eddies in the bowl and this could affect separation adversely. This problem has been
referred to the maker of the centrifuge. The other factors are:

• The temperature: This must be kept at 95°C.

61
• Variable feed rate: The abrupt variations in the amount of crude oil fed into the
centrifuge are not conducive to efficient separation
• Boiling of crude oil and period of ebullition. Table 2 gives the residual amount of
oil in NOS (a) versus the time during which crude oil is boiled and also (b) versus
dilution.

TABLE 2. EFFECT OF DILUTION AND BOILING TIME ON THE OIL CONTENT ON NOS
(RESULTS EXPRESSED IN % OIL ON NOS)
Dilution Not boiled Brought to Boiled for Boiled for Boiled for Boiled for 100
(%) boiling 15 min 30 min 90 mint to 180 min
0 55 - - - 30 -
100 22 11 11 11 12 43
200 22 - 20 27 - -

The 100% dilution appears to lead for getting the best results. It seems also
that boiling either through direct steam injection on by means of steam coils is
sufficient to induce a satisfactory extraction of oil. In the above cases involving
100% dilution, boiling was carried out either by steam injection or by steam coil (12%
and 11% oil on NOS respectively). Each result is the average of eight tests carried
out on samples taken whilst the machine was operating at three different throughputs.

The wear of the continuous discharge sludge centrifuge appears to be less

severe than in the case of the previous one. The nozzles, although made of special
metal; have to be renewed periodically. In a comparison between the resistance to
abrasion of nozzles made of two different metals it was established that tungsten
carbide is eight times as durable as satellite (cobalt alloy).

In the case of crude oil containing a large amount of sediments, the strainer
placed in the feeding chamber displayed a tendency to clog up although the size of the
perforations were larger than that of the sediments.

The screen can be cleared by a spray of water or simply by applying slight

vibrations to the chamber. At the time of the trial a device to impart vibrations to the
strainer was being designed.

62
 The continuous discharge sludge centrifuge of the type under discussion
presents a number of advantages in respect of automatic operation. After starting the
machine and adjusting the self regulating make up water addition, all that is required
is to ensure that crude oil does not overflow from the feeding chamber. By fitting an
automatic float valve to maintain a constant level the machine operates by itself and
requires no supervision. Several factors may however perturb the machine operation;
they are as follows:- Insufficient crude oil temperature, insufficient pressure of the
make up water (at least 3 maters) and clogged discharge nozzles.

The last point is important. It has been observed that as soon as one nozzle
gets blocked, sediments accumulate in that branch of the star and consequently eddies
occur in the bowl. This induces abnormally high losses of the oil in the discharged
effluent.
In order to avoid them, the strained crude oil must be protected from exposure
to sources of contaminations. Moreover, a quick response indicator must be fitted to
signal a drop in the throughput of the nozzles. Such an indicator may consist of the
bell controlled by the time of filling of the recording basculators. The inertia of such
a system is low since it is at worst equal to the time taken for one of the basculator
compartments to fill up. At Mongana, the time to fill up one section was 40 seconds
when operating the centrifuge at 5.4 t hr-1 . The clogging of one of the nozzles was
therefore detected by the increase in the time required to fill up one compartment (48
seconds).

A number of problems specific to the machine have still to be studied. Among

these:-
• reason for the sudden emulsifications of some oil
• effect on oil removal of plates with perforations close to the center
(lengthening of the zone of oil extraction);
• gurgling sounds detected in the bowl; and
• slow and recurring variations of the machine capacity.

63
 A flow meter was fitted on the upper water pipe and a tachometer was also
provided. They were not standard equipment but were however, necessary to
maintain efficient control of the machine. The centrifuge can be converted into a
purifier by increasing its speed of revolution, charging the plates and reversing the
direction of the pumps. Difficulties are experienced however as a result of these
modifications.

The Star-Rotor Sludge Centrifuge (Stork):

This machine discharges effluent continuously as the previous centrifuge but operates
without a pump. The evacuation of oil from the bowl is controlled through a valve
placed on the outlet pipe located at the centre of the bowl. Its disadvantage compared
to the previous machine is to yield oil containing more moisture and more impurities
(several percentage units against 0.7% moisture and less than 0.01% impurities); also
the absence of a regulator of the oil water interface. It may happen therefore that
through the throttling of the oil discharge, the bowl fills up with oil and the latter is
eventually discharged through the nozzles. The machine is particularly adapted to the
treatment of sludge or oily water. No make up water is required. The water content
of sludge is high enough. Its efficiency of separation is slightly lower than that of
bowl and plate centrifuges.

Compared to the intermittent discharge centrifuge (Titan) these machines offer

the advantage of being rugged, continuous and less prone to wear. Its operation
requires only limited supervision. The very principle on which it is designed
precludes its utilization as a purifier.

Settling Characteristics of Crude Oil - Study of the δ-Coefficient

Clarification losses occur in the sediments trapped in the centrifuge bowl and in solids
of the discharged effluent. In both cases, the loss consist of the “free oil”, which can
be recovered and of the ‘oil bound to the NOS’. Mthods are evolved to assess them
separately. They consist in the prolonged centrifugation in a laboratory machine of
the material to be analyzed. They made it possible to evaluate also the γ coefficient or
the centrifuge efficiency. The latter is solely governed by the amount of “free oil”
lost since the amount of oil bound to the NOS is practically constant.

64
 The efficiencies of three different types of centrifuges were determined and
was found to the close to 1 or at any rate higher than 0.99. The δ-coefficient or the
settling characteristics was determined in the case of the oil derived from various
types of fruit sprocessed according to various extraction techniques.

The settling characteristics are not constant. They are governed by the NOS
content of the crude oil and by the composition of the NOS. In the best possible
conditions, cellular debris are likely to retain 15 to 25% of oil, whereas the oil content
of the insoluble constituents of the NOS (fibre for instance) can be brought down to
approximately 10%. As regards the water soluble constituents of the NOS ( pectin for
instance), their oil content after centrifugation is close to nil.
As has been mentioned before, half of the constituents of the NOS are soluble
in water or at least can be solubilized. The amount of oil bound to the NOS is
therefore close to 10%. The settling capacity can therefore be established by
calculation. Its reliance has been established experimentally.

11. PURIFICATION

It consists in removing traces of impurity and a few tenths of percentage unit of water
still present in oil after static settling or centrifugal separation. Four different
machines were tested, three with bowl and plates revolving at 6000 rpm (de Laval,
Titar, Melotte) and one with a spindle shaped bowl revolving at 15 000 rpm
(Sharples).

The separation of the solids is equally effective in any of these four machines
with an output ranging from 350 to 3500 kg of oil per hour. A slightly brighter oil
appears to be derived from the machine with plateless bowl in which accelerations
higher than 10 000 g are applied.

The chief difference between the machines is the amount of solids that can be
retained in the bowl and the eventual dehydration that may occur therein.

65
 Two of the centrifuges can hold 2 kg of wet sediments i.e 0.4 kg of dry solids
in the bowl (Melotte and Sharples). These two machines do not permit direct
dehydration. The other two provide for dehydration, the first through the natural air
draught created by the rotation of the bowl and the second through provision of fan
since natural ventilation is not sufficient. The advantage of the latter machine is to
eject the sediments automatically through the operation of a suitable valve (Titan).

All these centrifuges yield purified oil containing less than 0.01% impurities,
which is the detection limit of the standard determination procedure and less than
0.35% of water. The moisture content can be reduced to about 0.05%, if the
centrifuges are used at low throughput.
Degumming
It is a well –known fact that crude oil contains substances of a complex nature,
which are soluble or at least dispersible in freshly produced oil but which precipitate
under certain conditions, particularly through ageing of the wet oil. These substances
are described in the palm oil industry as “mucilage”. They consist mainly of
phosphatides. Some oils (soya bean oil for instance) contain exceptionally high
amounts of mucilage. Before use, they should be suitably treated in order to remove
them. The mucilage content of palm oil is very low, hardly more than a few
hundredth of a percent. A number of users of palm oil have however, complained
about the deposit found in oil which they regard as just another impurity similar to
sand, fibre and organic debris, which are normally present in the oil.

Carefully controlled shipments of oil, in which strict conditions of cleanliness

were achieved, failed to induce a marked improvement. In the course of storage and
transport, precipitates materialized at the bottom of the land or ship tanks.

These precipitates are described as “impurities of maturation”. Users of palm

oil eliminates mucilage in the course of the alkaline refining in the case of utilization
as a basic material for margarine production or by treatment with surfactants in the
case of industrial utilization (metallurgy and plating).

66
 An attempt was made to separate the “impurities of maturation” into basic
constituents. The oil was mixed with water at a high temperature (90°C). The
resulting substance consisted mainly of soap. Table 57 gives the relevant information.

Industrial techniques of mucilage removal (degumming) are numerous. They

are covered by a number of patents (30, 31, 32).

The industrial techniques can be classified as follows:

• degumming by alkaline treatment;
• degumming by acid treatment;
• degumming by organic and mineral salts;
• degumming by absorption;
• degumming by physical methods (ultrafiltration, passage through an
electric field); and
• degumming by aqueous treatment.

The last of the above methods was implemented at industrial scale at Mongana
although to our knowledge it has never been used form palm oil before.
The involves the following steps:

• precipitation of the mucilages by aqueous treatment;

• separation of the precipitate and possible; and
• the purification of the precipitate.

67
 TABLE 3. IMPURITIES OF MATURATION

FFA 1.51
Soap expressed in g for 100 g of FFA 2.92
Ether extract (molecular weight 256)
13.85% Nitrogen: 0.53% as proteins 3.44
Phosphorous 0.11
Ash 3.01

100% 10.99
Soap expressed in g for 100 g of FFA 38.4
(molecular weight 256)
Not readily hydrolysable soap 4.5
FeO 3 9.10
SiO 2 3.51
Extraction Ash 30.9% CaO 0.60
Residue MgO 0.00
86.15% Residue 17.69

Dry mucilage dissolve or are dispersible in oil. They swell under the effect of
moisture absorption and form substances, which agglomerate and become insoluble in
oil. As a result of the high moisture content, their density is higher than that of oil.

Mucilage can be made to absorb moisture through the following processes:

• intimate mixing of purified oil with water;
• addition of water during the centrifugal extraction of the digested
mash;
• centrifugation of oil coupled with addition of water in the machine
using a suitable gravity disc;
• steam injection using an ejecto-mixer; and
• centrifugal straining of a water and oil mixture through a fine strainer.

Several of the above methods are continuous.

68
 The time of contact between oil and water varies from one process to another.
Strict control of temperature must be achieved failing which the hydrated mucilage
can re-disperse in the oil.

The separation of the precipitate can be made by static settling or better still
and quicker by centrifugation. In that case, the precipitate can either be retained in
the centrifuge bowl or eliminated together with excess treatment water. The raw
mucilage can be partially dehydrated by centrifugation.

Unlike some vegetable mucilage, such as the lecithins of soya bean and
groundnut, those of palm oil after exposure to air and are not hydroscopic. They
consist of waxy white colored powder, which keeps indefinitely.

Degumming modifies the physical properties of palm oil, particularly as

regards the characteristics of solidification. It does not seem to affect bleach ability
but leads to markedly lower Wesson loss. It may quite possibly have an effect on
the oil resistance to oxidation and consequently in an indirect manner on bleach
ability. It should be noted that the drying of oil to less than 0.1% moisture as is
required to avoid acidification totally prevents the separation of maturation impurities.

12. CLARIFICATION OF SCREW PRESS CRUDE OIL

The clarification is organized according to the flow sheet of Figure 1. Crude oil is
collected in a tank where dilution with hot water takes place. Dilution is continuous
can be controlled by an appropriate equipment (double tank basculator). The diluted
crude oil is brought to boiling point by live steam injection. It is then strained through
a 20 mesh rotary screen (3000 rpm). The strained material is then fed into a large
capacity sand cyclone and recycled from 2 to 3 times through it with the overflow
returned to the strained oil receiving tank. That tank is provided with steam injection.
All steam injectors are equipped with a silencer, which reduced noise and also
vibrations.

69
 The diluted crude oil is centrifuged in a bowl and plates centrifuge with
continuous discharge of the solids. The make-up water is provided by a constant level
tank fitted with a heat exchanger controlled by a thermostatic steam valve. The
amount of effluent discharged by the machine is recorded by a basculator. The
amount of make-up water is measured by a flow-meter of the mercury column type.

The instantaneous throughput of the crude oil is therefore known at all times.
Clarified oil is collected in a calibrated tank. It is then heated up by a thermostatically
controlled device and passed through a centrifugal purifier and finally to a drier after
which it is pumped into the storage tank.

Clarification and purification are completely automatic and continuous and

only require supervisory labour.

De-hydration and Re-hydration of Oil

Experiments on the spontaneous hydrolysis of palm oil have shown that the reaction
is of the type of the common hydrolysis; the so-called catalyzed monomolecular
hydrolysis; that is, the formula of the instantaneous speed of reaction does not include
a factor linked to the moisture concentration so long as the latter is close to saturation.

However, in practice, if the moisture content is appreciably below the

solubility limit, the speed of reaction of the hydrolysis is considerably reduced.
Practically, when moisture content reaches the level of 0.1% and if there is no
moisture available to compensate for the water utilized in the hydrolysis, it may be
considered that the acidification process is almost completely stopped. This is due on
the one hand to the fact that for moisture contents around 0.1% the hydrolysis
proceeds at a velocity markedly lower than that prevailing at or close to saturation
level and, on the other hand, to the fact that any tendency to hydrolysis entails a
depletion of moisture and consequently a slower reaction speed.

The problem of oil storage is therefore primarily one of drying and secondly
one of preventing the absorption of atmospheric moisture.
The study which has been undertaken consists of the following:-

70
 • study of the solubility of water in palm oil;
• determination of the vapour pressure of the dissolved water;
• drying through dry air bubbling;
• industrial drying of oil or dehydration;
• hygroscopic characteristics of the oil that is the rate of moisture
absorption in humid surroundings; and
• speed of moisture absorption under industrial conditions, i.e. re-
hydration.

These points are examined in detail below:-

Solubility of Water in Oil

This has been determined in relation to temperature, free fatty acid content and free
hydroxyl radicals. The determination is carried out by centrifugation of the oil to
which has first been added an excess of water. A special container is used. The water
content of oil is determined after prolonged centrifugation. In fact, the solubility
corresponds to the asymptote of the dissolved water contents recorded after multiple
centrifugations.

The determination of water in oil is carried out using acetyl chloride (Kaufman
& Funeks). The solubility curve of a few samples of oil is given in Figure 1. The
solubility increases with increasing FFA content and with higher temperature.
Comparative tests on refined oil to which fatty acid has been added and on naturally
acidified oil, that is possessing a high hydroxyl value, show that the free OH radicals
play a part in the solubility of water in oil but a lesser one than that of temperature or
free fatty acids.

The determination of the solubility of water in oil can only be carried out
above a temperature of 40°C. In order to determine the solubility of water in oils
which remain fluid at 0°C, corn oil at 0.28% free fatty acid and soya bean oil at 0.11%
FFA were tested. The results which are shown in Table 1 show that the pattern is the
same as for palm oil.

71
 TABLE 1. SOLUBILITY OF WATER AT VARIOUS TEMPERATURE
EXPRESSED IN % ON OIL)]

Oil Temperature
0°C 40°C 80°C
Corn oil 0.145 0.255 0.375

Soya bean oil 0.090 0.200 0.290

MOISTURE
CONTENT

0.45

0.40
6.44%
FFA
0.35
2.43%
FFA
0.30
0.19%
FFA
0.25

0.20

0.15
40 o 50 o 60 o 70 o 80 o
Temperature

Figure 1. Solubility of Water in Palm Oil Versus Temperature and Initial FFA
Content

The examination of the various results makes it possible to state tentatively

that the solubility of water in vegetable oils is governed by the following equation:
S = A + B (FFA) + C
Where,
S = the solubility in g % of water;

72
 A = a constant specific to the oil considered;
B = the factor of increase for each percentage unit of FFA;
C = the factor of increase for each degree of temperature;
FFA = free acidity in g % of palmitic acid; and
T = temperature in degree centigrade.

In the case of palm oil of Congo origin, particularly within the range of temperature
50°C to 80°C and the range 0% to 7% FFA, the above equation is expressed by the
following:
S = 0.198 + 0.0112 (FFA) + 0.00467 (t-50)

The equation enables an assessment to be made of the solubility in routine

conditions for a naturally acidified oil. In other words, it provides an estimate of the
maximum moisture content likely to be found in oil at the outlet of a perfectly set
industrial centrifugal purifier in which no dehydration take place as a result of
evaporation through contact with air.

It is necessary to point out that the two equations are only rough
approximations. They are however sufficiently accurate for routine practice provided
they are used within the specified range of temperature and acidity.

In particulars, the affect of temperature must be checked through the use of the
general law on solubility equilibrium:

d.1n S = H
dt RT2

where
S = Solubility
T = Absolute temperature
H = Heat of solubilisation
R = Constant of perfect gas

73
 By integration and conversion to decimal logarithm the following is obtained:
Log. S = - K 1 + C
T

By plotting log S against the reciprocal of temperature (for two values of T), a
straight line is obtained, which makes it possible to read off solubility at any
temperature, provided H remains fairly constant over a wide range of temperature.

Vapour Pressure of Water Dissolved in Palm Oil

The need to dehydrate oil to improve its keep ability makes it necessary to
have a detailed knowledge of the vapour pressure of dissolved water. The knowledge
permits to establish the feasibility of industrial drying.

The determination of the water vapour pressure in oil has therefore been
undertaken. The apparatus (Figure 2) consists of a 250 cc round flask equipped with a
mercury manometer and fitted with a lateral tube which is sealed after the flask has
been completely evacuated. The flask is then immersed in a thermostatically
controlled water bath accurate to the 1/10th of a degree. The changes in mercury level
in the monometer are recorded. The moisture content is determined by the acetyl
chloride method (33) at the end of a series of recordings at various temperatures. The
results are corrected for the following:
• the residual air estimated by a measurement carried out at 0°C on the
assumption that at that temperature the atmosphere is saturated with
moisture. (in our tests, the correction was always lower than 55 mm of
mercury); and
• the density of mercury at various temperatures (the correction is very
small; of the order of 1 mm of mercury for the higher temperatures).

The results of the determination of moisture content of oil can be accepted

without correction for the various temperatures. The accuracy is of the order of 1%
when the volumes of the vapour phase and the lipid phase are respectively 50 and 200
cc. The eventual correction is smaller than the titration accuracy.

74
 The results are shown in Table 2 and are plotted in Figure 3 and 4 (vapour
pressure against moisture content). The solubilities as determined in Section 1, taking
the vapour pressure of free water as corresponding vapour pressure, are also plotted
on the graphs.

TABLE 2. VAPOUR PRESSURE IN MM OF MERCURY VERSUS

TEMPERATURE.

50°C 60°C 80°C 80°

% Moisture a) Oil at 6.44% FFA

Water alone 92 mm 149 mm 234 mm 355 mm

0.16% 52 mm 79 mm 116 mm 157 mm
0.10% 37 mm 51 mm 74 mm 99 mm
0.01% 4 mm 6mm 8 mm 12 mm

b) Oil at 2.44 % FFA

0.12% 47 mm 67 mm 88 mm 116 mm

The results follow fairly closely Henry’s law: “The amount of a gas of low
solubility, which dissolves in a given mass of liquid at a defined temperature, is
directly proportional to the partial pressure of the gas”.

The makes it possible to establish “a priori” the equilibrium moisture content,

that is the maximum limit of drying that may be attained with air at a given
temperature and a known degree of hygrometry. This is because the equilibrium
moisture content is equal to the solubility multiplied by the hygrometric degree of the
air. A mathematical expression is as follows:
H3 eq t = StKt
Where
Heq t = equilibrium moisture content at t o
St = solubility at temperature t o
Kt = bygrometric degree if air at t o

75
 300 mm

250 ml

Figure 2. Apparatus for the Determination of the Vapo ur Pressure of Water Dissolved in Oil

WATER VAPOUR
PRESENT IN mm
MERCURY

400 80 O

300 70 O
OIL AT 6.43 % FFA

LIMIT OF SOLUBILITY
200 60 O

50 O
100 Solubility measured
water pressure

0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40

MOISTURE CONTENT % →

76
 WATER VAPOUR
PRESENT IN mm
MERCURY

400 80 O

OIL AT 2.44 % FFA

300
70 O

200 60 O

50 O
SOLUBILITY
100 MEASURED IN
WATER
40 O PRESSURE

0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40

MOISTURE CONTENT % →

Figure 3 & 4. Vapour Pressure of Water Dissolved in Oil within the Concentration
Range from Nil to Solubility Limit.

For technical reasons, no determination of solubility and vapour pressure was

carried out at 100°C oil within the FFA range 1 to 7% reaches equilibrium for air with
water vapour pressure of about 30 mm of mercury (maximum in Congo) when the
moisture content of the oil is within the range 0.017 to 0.020%. The latter must be
considered as the limit obtainable for oil at 100°C and air in the Congo. It could be
lowered (which does not seem to be of practical value) by increasing the temperature
of oil or through desiccation of air.

13. Study of the Quality and Characteristics of Oil

General
In the preceding chapters the conditions required to produce a “pure oil”, that is free
impurities and moisture were examined. Other criteria make it possible to assess the
quality of crude palm oil. The following may be listed among others:
• FFA content;
• Degree of oxidation;

77
 • Bleach ability;
• Refining loss;
• Transparency;
• Mucilages which precipitate of settling (particularly in the presence of
water);
• Heavy metal content;
• Unsaponifiable matter content;
• Saponification value;
• Plasticity at various temperature levels below melting point;
• Unsaturated acids content; and
• Flash and flammability points.
Before going further into the detailed study of these criteria, some typical
values are given below for average oil of good quality.
• FFA content: as low as possible. Normally between 1% and 2%
except for oil used in metallurgy for which the optimum value seems to
lie within the range 4% to 8% (34);
• Degree of oxidation: As low as possible. In terms of peroxide value,
lower than 2;
• Bleachibility: Residual colour very faint. No green of grey blue;
• Refining loss: As low as possible. It is governed by the FFA and the
mucilage content;
• Heavy metal content: As low as possible;
• Unsaponifiable matter: As low as possible in the case of oil used in tin
plating (34);
• Saponification value: As high as possible for oil used in cold rolling of
metal;
• Transparency: As high as possible;
• Products of maturation content: As low as possible.
• Plasticity: Primarily must be consistent.
• Unsaturated fatty acids: Low for oil used in thin plating (35); and
• Flash and flammability points: Very high for oil used in thin plating
(36).

78
 Finally, the point forcefully made by most users is the need for consistency in
physical and chemical properties. Very often, the absolute value of one criterion or
the other such as plasticity or saponification value is of little importance by the
producer must be in a position to guarantee that these characteristics will remain more
or less similar from one shipment to another.

It should be pointed out again that the impurities content should be lower than
the sensitivity threshold of the determination, that is 0.01% and that the moisture
content should be appreciably lower than 0.10%.

14. FFA CONTENT

Acidification during processing

Oil contained in the unbruised, ripe and fresh fruit has an FFA as low as 0.25%.
Industrial scale processing of such crop lead to oil with FFA 0.35%. Through
sterilization of the bunches it is possible to produce, industrially, oil at 0.8% or 0.9%
FFA provided handling of crop is reduced to the minimum.

Processing itself accounts but for a very small increase in FFA. The
spontaneous auto-catalytic hydrolysis which will be studied in a further section
permits to calculate the magnitude of the FFA increase during storage at high
temperature. In the most unfavourable conditions during processing, the oil is
maintained at 140°C for one hour (sterilization) and at 100°C during 24 hours (batch
clarification). On the assumption that the value of the rate of the hydrolysis reaction
which will be discussed later for a 1% FFA oil is 0.11% during sterilization and
0.16% for the subsequent treatment, the total increase in FFA will be 0.27%.

Composition of the free fatty acids

The characteristics of the free and combined acids have been determined for oils with
FFA 4%, 9% and 44% respectively. No significant difference was found as regards
iodine value, molecular weight and melting point. The inference is that free fatty
acids have roughly the same composition as the fatty acids combined to the glycerides.

79
The hydrolysis which takes place in the fruit as well as during the storage of the oil
itself is therefore not a selective process.

Furthermore, these results show that free fatty acids are solely the end
products of a non oxidative hydrolysis without molecular chain splitting. May
authors yet regards the reaction as an oxidative process.

It is worthy of note that for naturally acidified oil there is a close correlation
between the acid value and the hydroxyl value. It may be observed as shown in the
hydrolysis representation given in Figure 1 that the formation of OH ions is
concomitant to that of COCH. In the case of fresh fruits the hydroxyl value is high
that the acid value because of the presence at the moment of ripeness of small
amounts of mono and diglycerides. On the contrary, oil with high FFA contains a
certain amount of free glycerol which therefore explains an excess of acid value over
the hydroxyl value. The ratio of the acid to hydroxyl value for 3 types of oil is given
in Table 1.

TABLE 1. RATIO OF ACID VALUE TO HYDROXYL FOR VARIOUS OILS

% FFA Acid value Hydroxyl CO2 H

value OH

Low FFA oil from fresh fruit or 0.7 1.5 4.9 <1
bruised fruit processed without
delay.

Average FFA oil or oil obtained 6.0 13.2 14.3 1

from bruised fruit processed 10
min to 30 min after bruising.

High FFA oil 35.0 79.6 30.0 >1

Formation of free fatty acids

Natural acidification
General
Several years ago it was observed that the FFA content of oil increases on storage
after production. The mechanism had never been studied and most authors who had

80
dealt with this question had ascribed it to the effect of lipolytic enzymes either present
in the fruit pericarp or produced by microorganisms (37) or to the action of rancid
evolution of hydrolytic origin (38).

Other research workers mention however hydrolytic reactions due to the

presence of impurities such as flour, products of cellular decay, mucilages, and also
water (39, 40, 41), these products being culture media a for the development of
lipolytic microorganisms. As will be seen in a further section dealing with
biochemical acidification, the hydrolysis has been investigated and elucidated.

In an investigation (42) Vanneck and Loncin had concluded that the

hydrolysis observed in practice was neither of enzymatic nor of bacterial origin and
that availability of water is indispensable, also that the FFA content affects the
velocity of the hydrolysis. The study was continued in detail to show that the reaction
may be described by the following equation:
dA = KA (100 – A)
dt ( 100 )

or in simplified form : dA = kA
dt
where
A = % FFA content
T = time (generally expressed in number of periods of 10 days each)
K = reaction constant
By integration the formula becomes:
K (t 2 – t 1 ) = log A2
2.3 A1
The hydrolysis reaction constant has been determined for natural and synthetic
palm oil (see appendix 3).
The synthetic oil used in the experiments described hereafter had an FFA of
0.05% and a hydroxyl value of 3.5.

Experiments on natural oil

The effect of the following factors has been studied:
• Origin of the oil;

81
 • The concentration of H ions in the aqueous phase;
• The presence if various impurities in the oil;
• The initial acidity;
• The addition of alcohols;
• The addition of various inhibitors; and
• The moisture content.

150 Concentration/ Corresponding 40

140 (mg/150 g) % FFA

130 35

120 % FFA
110 30

100

90 25

80 TRIGLYCERIDES

70 20

60

50 15

40 DIGLYCERIDES

30 10

20 MONOGLYCERIDES

10 5

10 20 30 40 50 60 70 80 90 100 110 120

Days
Figure 1. Variation of the constituents of oil during hydrolysis at 70°C.

Evolution of acid and hydroxyl values in the course of hydrolysis

Time (in day) 0 6 20 35 61 82 92 100 115
FFA % 4.46 5.24 7.42 10.7 18.6 26.4 31.1 35.8 40.6
Acid value 9.2 10.9 15.4 22.2 38.6 54.8 64.5 74.2 83.3
Hydroxyl value 8.3 10.2 15.6 22.2 39.7 52.25 58.2 60.1 60.0

82
Experimental on synthetic oil
The effect of the following factors has been studied:
• The addition of lecithins;
• The addition of soap of metals;
• The addition of palm oil unsaponifiable matter;
• The addition of surfactants;
• The addition of various organic substances, (pectin, filter paper, casein);
• The addition of various mineral salts;
• The carotenoids;
• The initial acidity;
• The nature of the free fatty acids; and
• The oxidized fatty acids.

It results from the tests that: (43)

In the presence of an excess of water and at a given temperature, the free fatty acids
already in the oil constitute by far the most important factor in the hydrolysis of the
oil. The reaction proceeds as an auto-catalytic process, that is at any time in the
range of low acidity the instantaneous rate of the hydrolysis reaction (as measured by
the amount of fatty acid appearing per unit of time) is more or less proportional to the
concentration in free fatty acid at that very moment.

The hydrolysis reaction takes place in the homogeneous phase using the water
dissolved in oil.

None of the compounds subjected to test possesses a catalytic action

comparable to that of the free fatty acids. Only the soap of heavy metals and
particularly that of chromium appears to exhibit the ability to speed up slightly the
process of acidification of the oil which already contains free fatty acids.

The various fatty acids with 16 and 18 atoms of carbon affect the hydrolysis
process virtually in the same manner whatever their degree of unsaturation or even if
they possess hydroxyl radicals (ricinoleic acid). For short chain fatty acids (with 12

83
and particularly 4 carbon atoms) the intensity of the catalytic effect is intermediary
between that which may be calculated in percentage by weight and in molar
percentage respectively.

Unlike fatty acids, mineral acids do not possess an ac idifying affect. This is
probably due to the almost total insolubility of these compounds in oil at the
temperature of the test (60°C). The naphtyl  sulphonic acid which is soluble in oil
has, on the contrary, a marked catalytic action (more marked than that of the fatty
acids evolved from the oil).

It is generally believed that palm oil undergoes hydrolysis more readily than
other oils before as well as after extraction. In order to ascertain this point, other oils
were placed in the same conditions as palm oil. The experiments showed that the
hydrolysis of coconut oil, ground nut oil and castor oil is very similar to that of palm
oil and retains its auto-catalytic characteristics. In the specific case of coconut oil,
with shorter molecular chains, the reaction constant k is slightly high than that of
palm oil.
On the contrary, methyl esters of palm oil subjected to storage are hydrolysed
according to a different law. The mount of FFA formed in the course of time is
simply proportional to that time and is no longer governed by the FFA content Figure
2.

Kinetics of spontaneous hydrolysis

Tests have shown that the reaction contents k is highly affected by temperature. It
may be accepted that its value approximately doubles for every 10°C increase.
The average of several hundred determinations is given in Table 2.

84
 TABLE 2. VALUE OF THE VELOCITY CONSTANT VERSUS TEMPERATURE

k °C k log. k
37 0.025 2.39
50 0.051 2.707
60 0.125 1.097
70 0.288 1.370
80 0.505 1.703
100 1.48 0.17

Figure 2. Hydrolysis of palm oil at 37°C and 60°C and of methyl esters of palm oil.
These results are plotted in Figure 3 below.
70 % FFA

60

50 OIL AT
6 60 O C

40

30

20 METHYL ESTERS
OF OIL
10 OIL AT 37 O C

0 40 80 120 160 200 240 280

Figure 3. Value of “k” in relation to temperature.

85
 Log K
1.58 0.2
1.00 0.0
0.631 1.8
0.698 1.6
0.251 1.4
0.158 1.2
0.10 1.0
0.065 1.8
0.040 2.6
0.025 2.4
0.016 2.2
30 40 50 60 70 80 90 100

The above values of k are valid over the whole range of temperatures by only
for relatively low acidities. This is due to the fact that the formula.
dA = kA
dt
applies only for low values of A.

If the hydrolysis is allowed to proceed, that is if A is allowed to increase, an S

shaped curve typical of equilibrium reactions is obtained.

Such a curve is plotted in Figure 2 and applied to oil stored at 60°C. In

principle, it is admitted that is long as the FFA content does not exceed about 15% the
law is verified satisfactorily. An analogy exists between the reactions described
above and the industrial hydrolytic splitting of fats at high temperature.

Evolution of the glycerides during hydrolysis

Numerous authors have studied that evolution during the industrial fat splitting
process by hydrolysis. It proceeds as follows:

Triglycerides Diglycerides + fatty acids

86
 Diglycerides Monoglycerides + fatty acids
Monoglycerides Glycerol + fatty acids

Spontaneous hydrolysis takes place in a in similar manner at low temperature. It has

been investigated at 70°C. Monoglycerides are titrated with periodic acid (44), the
hydroxyl value by the international producer (45) and moisture by the Fisher reagent
in Figure 1. It may be observed that the amount of monoglycerides becomes
significant only when acidity exceeds 10%, also that there is no important release of
glycerol until the acidity of oil reaches some 20% FFA. At around 30% FFA, the
concentration of di di-glycerides ceases to increase; this is indicative that the speed at
which they are formed becomes equal to that at which they hydrolyse into
monoglycerides and fatty acids.

15. EFFECT OF MOISTURE

This has been studied on samples of oil stored in sealed tubes. It is virtually
impossible in that case to determine the value of k because a plot of logarithm of
acidity against time leads to curves having their concavity towards the t axis. The
apparent rate of the reaction decreases very quickly as the reaction proceeds.
Furthermore, aberrant results are recorded frequently owing to the very small amounts
of moisture to be determined. A few results are gathered in Table 5.
(Note: Please note that k = reaction constant, A = % FFA, t = time (generally expressed in number of
10 days each) as defined in part 16 of the Engineering Bulletin Issue 89)

In order to find out whether the stabilization obtained by dehydration was

governed by the FFA content of oil, samples of oil with different levels of acidity
were dried by bubbling of nitrogen and were stored in sealed flasks at 58°C. It was
observed that the hydrolysis reduces significantly less as the moisture content
decreases. No equilibrium is reached; the hydrolysis proceeds until all the moisture
has been taken up. The inhibition is therefore proportionately more important for oil
with high acidity than for oil with low acidity Tables 3 and 4.

TABLE 3. LOW FFA OIL

87
Time % FFA % FFA Moisture Calculated from the
determined by calculated for content found concentration of FFA
analysis saturated oil

0 0.98 0.98 0.11 0.11

6 0.98 0.98 0.12 0.11
36 1.16 1.48 0.11 0.08
49 1.27 1.72 - 0.06
81 1.55 2.50 - 0.06
136 1.73 4.78 0.07 0.04
183 1.97 9.06 - 0.03
214 1.99 10.55 0.5 0.02

TABLE 4. HIGH FFA OIL

Time % FFA % FFA Moisture content

determined by calculated for Found Calculated
analysis saturated oil

0 5.28 5.28 0.10 0.10

28 5.60 7.31 0.09 0.08
41 5.82 8.49 - 0.07
73 6.18 12.35 - 0.05
128 6.40 23.30 0.04 0.03
175 5.51 40.30 - 0.02
205 6.44 57.20 0.04 0.01
223 6.57 73.00 0.02 0.006

In the experiments described above, oil with moisture content 0.10% to 0.11% was
used. The inhibition is consequently very marked.

It may be useful to know from what level of moisture content this inhibition
takes place. To that end, the comparison was made between the acidification of two
samples of oil saturated with moisture. One was continuously brought back to
saturation whilst no water was added to the other.

88
 TABLE 5. ACIDIFICATION OF PARTIALLY DEHYDRATED OIL

Time (in days) Final

Sample % 0 6 12 18 25 29 35 moisture
number moisture content
(calculated)
1 0.205 7.35 7.42 7.95 8.11 8.25 8.20 - - 0.14
2 0.265 7.35 7.80 8.41 8.81 8.90 0.24 9.20 - 0.13
3 0.465 7.35 7.77 9.08 9.55 9.90 10.70 10.32 - 0.23
4 0.630 7.35 7.98 0.00 10.05 10.25 11.10 11.20 - 0.36
- 0 5 11 19 27 33 40 43 -
5 0.110 2.02 2.12 2.27 2.30 2.38 2.38 2.36 2.39 0.08
6 0.175 1.98 2.20 3.34 2.45 2.90 2.82 2.97 2.93 0.10
7 0.145 3.10 3.37 3.46 3.54 3.76 3.79 3.78 3.81 0.09
8 0.195 2.01 2.27 2.47 2.68 2.99 3.04 3.26 3.30 0.10
9 0.100 3.02 3.30 - 3.40 3.46 - - - 0.07
- 0 7 12 15 19 27 - - -
10 0.060 7.90 8.06 8.26 7.86 7.91 - - - 0.06
11 0.175 7.90 8.24 - 8.61 8.97 - - - 0.10
12 0.280 7.90 8.86 8.33 - 9.75 10.70 - - 0.08
13 1.140 7.90 8.40 8.90 10.52 10.70 12.95 - - 0.80

It is rather difficult to pinpoint the time at which the inhibition starts, at least
for low acidity oil. It is however, readily noticeable that for a moisture content of the
order of 0.16% the hydrolysis undoubtedly slows down. If the inhibition is described
as the ratio of the reaction rates in dehydrated and saturated medium respect ively, it
may be observed that a value of 0.5 is recorded when moisture content is within the
range 0.08 to 0.10%. Figure 2 and 3 illustrate the acidification process taking place
in the case of oil permanently saturated with moisture and in the case of the same oil
saturated at the beginning of the experiment but allowed to dehydrate itself in the
course of time.

Oil with free fatty acidity of 1.35% was used in the experiment of Figure 2.
Figure 3 pertains to oil at 5.6% FFA.

Figure 1 gives a plot of the ratio of the speed of acidification of dehydrated

and moisture saturated oil versus the moisture content of the oil. Taking into account
the lack of accuracy of the moisture content determination, it may be considered that
the instantaneous speed of hydrolysis remains constant when moisture content ranges
from the saturated limit to approximately half that value.

89
 From that point, the speed of hydrolysis of partially dry oil is described
approximately by

da = k.a.c
dt

where c = moisture content

solubility of water in oil

In practice, when moisture content is of the order of 0.1% the process of

acidification is hardly noticeable, first, as a result of the slowing down of the
hydrolysis reaction and second because the hydrolysis process further reduces the
available moisture and therefore the reaction speed.

Observed speed of acidification

Speed of acidification of oil saturated with moisture with= Increase in FFA% over a period

0.20 0.10
0

90
Figure 1. Observed Inhibition of acidification of de-hydrated low acidity oil

5 0.25

4 0.20

3 0.15

2 0.10

1 0.05
%FFA 1d ays 10 20 30 40 50 60 %
Moisture

Days

Figure 2: Hydrolysis of partially de-hydrated oil

FFA % %
11 Moisture
High Acidity oil

10
0.25

9 Moisture (calculated) Moisture saturated Oil- FFA 0.20

8
0.15

Partially De-hydrated oil

7
0.10

6
0.05
Days 10 20 30 40 50 60

Figure3: Hydrolysis of partially de-hydrated oil- continuation from 2

91
Effect of Hydrolysis Inhibitors
We have seen that the speed of the hydrolysis could be modified in two ways only,
either through dehydration (slowing the reaction speed) or through adjunction of acids
soluble in the oil (increasing the reaction speed).

It may therefore be stated that the removal of acid from the oil (neutralization
or distillation of the fatty acid) should lead eventually to a slowing down of the
hydrolysis reaction. The removal of acidity entails technical difficulties in the Congo.
The drying of oil, on the contrary, can be arranged at industrial scale using non
sophisticated equipment as has already been shown in Chapter V.

Research has however been undertaken to ascertain whether dehydration was

the only practical method of stabilizing the acidity of oil. Since the hydrolysis is an
equilibrium reaction, the shift of the equilibrium through the action of primary OH
groups has been studied. The inhibition effect of these substances (glycerol, methanol,
saccharose) is noticeable but not very marked, whether with or without an excess of
moisture (saturated atmosphere). Comparing the inhibiting action of methanol,
ethanol and glycerol on the hydrolysis, it has been observed that primary OH groups
appeared to be more active than secondary groups. An attempt was therefore made to
find substances having primary OH groups but more soluble in oil then glycerol. The
mono-substituted derivatives of glycerol of the type mono-byturine are not very active
in comparison with glycerol in spite of the increased solubility in oil. Ethylglycol and
the epicholorhydrine are slightly more active. With a view to increasing the solubility
of glycerol in the oil, chemicals were prepared from glycerol in which one or two
function were substituted (formation of epoxy function).

The monoethyl and monobutyl etheroxides of epoxyglycerol appear less active

than ethylglycol or epichlorhydrine. Other derivatives of glycerol were assessed.
Among these were diepoxyhexane and glycidol. The latter and the latter only,
exhibits a sharp inhibition effect. The effect goes even further in fact since
immediately after its addition to oil a decrease in the FFA content can be observed as
a result of re-esterification.
H - C

92
 O

H - C

Epoxy group

The effect of glycerol has not been studied in detail. It has been observed that
it acts through simple esterification of the primary OH group without splitting of the
epoxy bridge.

It appears to be the most interesting of the addition products not only because
of its activity but also because it is simply a product of dehydration of glycerol. To
some extent therefore, its use does not introduce an abnormal constituent into the oil.
Glycidol is prepared through the action of metallic sodium on glycerol
monochlorhydrate in the presence of ordinary ether. The reaction is as follows:

CH 2 Cl CH 2
O
CHOH + Na CH

CH 2 OH CH 2 OH

The chemical acts on oil of any acidity and at the rate of 0.5%, its effect is
sharp.

16. Mechanism of Hydrolysis

93
It has been pointed out the naphtyl sulphonic acid possesses an autocatalytic action
more intense than the fatty acids derived from the oil itself. Since that acid is stronger
than the fatty acids it can be assumed with a reasonable degree of probability that the
reaction is of the ordinary acid catalytic type but it occurrs in the lipid phase.

The catalytic hydrolysis of esters is considered as a chain reaction, which

features the fixation of a H + ion, the formation of oxonium. This in turn decomposes
into carbonium ion and a free alcohol radical. The carbonium ion yields a fatty acid
after fixation of one molecule of water and the release of on H + ion.

O O
ll +
R1 - C + H+ R1 - C - O - R (1)
|
OR H
ester proton oxonium

O
ll + +
R1 - C - O - R R1 - C -= O + ROH (2)
(2)
l
H
oxonium carbonium alcohol

O
+ ll
R1 - C = O = H2O R1 - C - OH + H+ (3)

carbonium acid proton

The above hydrolysis reaction appears to follow a monomolecular

autocatalytic pattern. It has not been possible to establish a relationship between the
moisture content and the rate of hydrolysis. It is highly probable that the slowest part
of the reaction, that which governs the overall reaction rate, is the decomposition of
oxinium into carbonium, the latter becoming hydrated and then releasing a H+ ion. It
would be necessary to accept the fact that, at least within a certain range, the degree of
dissociation of the free fatty acids dissolved in oil remains more or less steady. This
would explain why the rate of reaction constant does not appear to the markedly
affected by the acidity.

94
Conclusions – Summary
The hydrolysis of oil in the presence of an excess of water exhibits the
characteristics of an autocatalytic reaction. It is not enzymatic. The reaction proceeds
in homogeneous phase at the expense of the water dissolved in oil. The reaction is
monomolecular, the limiting factor being probably the decomposition of the oxonium
ion. However, when the dissolved moisture content falls below the half saturation
mark, the reaction rate slows down considerably. In practice, it may be considered
that oil with moisture content less than 0.10% does not acidify to a significant extent.
Total stability can however be achieved only with complete dehydration.

The impurities of the oil do not have any effect on the hydrolysis. They may
trigger the reaction indirectly if they act as a culture medium for lipolytic micro-
organisms.

The effect of numerous compounds has been examined. Only acids soluble in
oil catalyze the hydrolysis. At equal concentration low molecular weight fatty acids
have a greater effect than those with long chain. The effect of temperature is very
marked. This is not specific to palm oil.

Some compounds can be esterified by the fatty acids of the oil. Glycidol was
observed to be the most active.

From the practical point of view, only the inhibition of the hydrolysis through
dehydration is of great interest. It is however, necessary to remark that low initial
acidity entails a marked drop in the rate of the hydrolysis reaction.

17. BIOCHEMICAL ACIDIFICATION

General
It was been observed that, in some instances, the acidity of palm oil in creased faster
than predicted by the autocatalytic law. In mills as well as on reception of oil at

95
Leopoldville, cases of abnormal acidification of purified oil have been recorded.
Furthermore, it has been noted that the addition of rotten kernels to palm oil or palm
kernel oil led to abnormal increases in acidity particularly when an extract had been
added.

The laboratory examination of these oils showed that abnormal acidification is

stopped when oil is sterilized at a temperature of 90°C; 60°C was even sufficient
sometimes. In those cases, bromoacetates have a inhibiting action, which may be
explained by the fact that these compounds act on micro-organisms and not on
enzymes. The processes of fast acidification often follow an irregular pattern. They
are usually not easily reproducible because the degree of dispersion of the aqueous
phase affects the reaction mechanism, the enzymatic or microbiological acidification
being necessarily a reaction taking place in a heterogeneous medium.

Instances of typical biochemical acidification have been observed on crude oil stored
at ambient temperature. Table 5 gives an idea of the intensity of the occurrence.

If hydrolysis had been of autocatalytic origin, the acidification process would

not have exceeded 0.1% FFA over 21 days (storage at ambient temperature that is
approximately 28°C).

TABLE 5. ACIDIFICATION OF CRUDE OIL IN THE COURSE OF TIME.

STORAGE AT EMBIENT TEMPERATURE (28°C)

Low pressure High pressure Centrifuge Digester Press

press press
Initially 2.82 2.75 3.05 2.81 3.53
After 3 days 3.29 2.89 2.93 3.46 3.83
After 7 days 3.41 3.05 3.62 4.28 6.61
After 14 days 4.43 5.17 3.89 5.06 7.28
After 21 days 6.28 7.53 4.71 5.66 7.77

In the above cases, the sterilization of crude oil followed by storage under
sterile conditions stop further acidification. This shows beyond doubt that the
increase in FFA is due to a thermolabile factor. Moreover, filtering the crude oil also
stops the process (separation of impurities). It may therefore be concluded that this

96
factor is active only in a richer and more balanced medium than just oil and water.
The factor can only be a lipase derived from the growth of lipolytic micro-organisms.

Search for Lipolytic Micro-organisms

Among culture media listed in technical publication, the following were selected for
various reasons:
• A standard gelatine medium, without sugar, containing 1% of tributyrin
emulsified by means of 1.5% Tween 80.
• A slightly modified Nile Blue gelatine medium.

The presence of a lipolytic micro-organism is detectable in the former though

the occurrence of a light colored zone around the colony and in the latter through the
deep blue colouration assumed by the lipolytic colonies.

A further test based on the hydrolysis of a solution of phenolphalein dibutyrate

is described in technical publications. This test, which has been checked on
Pseudomonas Fluorescens has yielded aberrant results when used on the aqueous
phase of the crude oil and on slurries of fresh fruit prepared in a turbo-mixer.

Another method which consists in shaking purified oil with a culture of micro-
organisms has not led to significant results.

Finally, a method which gives particularly significant results consists in

inoculating sterile crude oil from a continuous press with the strain to be tested. The
test was carried out on approximately 20 organisms isolated from infected crude oil.
The micro-organisms included 4 yeasts, 4 spore bacteria, 8 non spore bacteria and 8
fungi.

Of the 12 bacteria strains, only 3 (probably of the same species) gave a

positive test with Nile Blue culture medium and hydrolysed the phenolphthalein
dibutyrate. They appear unable to proliferate on crude oil or to hydrolyse it. In
view of the almost certain presence of lipase and of these bacteria in oil which acidify
rapidly it would have been desirable to study the latter in more detail.

97
 However, one of the isolated fungi is particularly remarkable with regard to its
lipolytic activity. On “potato agar” medium it appears in the form of slightly woolly
white colonies, which branch out radially from a focal point.

In the “Mongana” liquid medium, the composition of which is given in

appendix, the fungus produces a veil like colony, a ring and a blur. The microscopic
examination shows radially growing filaments, which were grouped in the early stage
but which sporulated rapidly on ageing. The spores fall out and in the free state, look
very much like large size yeasts.

The colony did not assume a blue colour in the Nile Blue culture medium.
The phenolphthalein dibutyrate test is positive and the inoculation of sterile crude oil
gives rise to rapid acidification which does not leave the slightest doubt on the role of
the fungus in similar cases encountered under routine conditions. For instance, a
sample of crude oil with initial 1.6% acidity was inoculated and showed an increase to
7% FFA after 3 days and 19.8% FFA after 21 days. This experimental acidification
has been repeated several times. The Commonwealth Mycological Institute, Surrey,
England identified the fungus as Goetrichium Candidum Link.

This fungus which was isolated from a batch of crude oil exhibiting proneness
to rapid acidification was identified in Petri dishes and isolation plates on which were
grown fungi collected from the inner side of the roof over an oil clarification station.
The rood had been soiled by projections of crude oil from a settling tank. The oil
produced in that particular factory (Mombessa) often underwent abnormally intense
acidification (2% during transport from factory to Leopoldville).

Another yellow fungus (Mucor) which turns black on sporulation is slightly

lipolytic. It was isolated from mouldy fruit and appears to be a very common
infestation in Mongana. A slight acidification of crude oil was shown to take place.
The seeded oil had an initial FFA of 1.6%. The acidity had increased to 3.4% after 21
days storage at ambient temperature. Its lipolytic activity is therefore considerably
lower than that of the Geotrichium strain.

98
Orange Fungus of the Empty Bunches
The fungus which covers sterilized empty bunches exposed to air for a few days with
a powdery orange colored layer is well known. The growth starts on the spike lets. A
sample was isolated on gelatin medium containing 10% o milk serum. The
proliferation is more rapid at 37°C than at 25°C. After 12 hrs at 37°C there appears a
white mycelium without sporangium. After 21 hrs at that temperature there appear
ramified, white, non separated macroconidies. The macroconidies grow in a direction
perpendicular to the culture medium. Their microscopic appearance is that of white
flakes. When the culture medium is exhausted, the spores assume a bright orange
colouration. Acidification tests were carried out by introducing fungus coloured
pieces of empty bunches into oil and also by stirring an aqueous extract of culture
intro the oil. The fungus has no lipolyitc activity.

Lipase of the Fruit

The lipase of the oil palm fruit is highly active but it has not been possible to prepare
an extract of the fruit pulp with marked hydrolyzing characteristics. As was started in
paragraph B, the pulp extract does not hydrolyse the phenolphthalein dibutyrate.
Even the thorough mixing of bits of pulp and purified oil in a turbo-mix does not
trigger hydrolysis of the latter.

Conclusions
It is absolutely certain that acidifications of microbiological origin can occur in oil
mills. Crude oil is particularly prone to that process but in all probability
inadequately clarified oil can equally be affected.
In practice, the clarification of crude oil must be carried out as soon as
possible after extraction. The oil should be “sterilized” through heating to a
temperature equal or higher than 90°C after clarification and purification. That level
of temperature is sufficient to destroy micro-organisms and the lipase they produce.

Finally, oil should be stripped of non-fatty substances normally found in all crude oils
(pectins and other carbohydrates), inclusive of water, with-out which micro-
organisms cannot proliferate

99
 18. OXIDATION OF OIL

Simplified Theory
Olefinic chains in contact with air undergo a slow oxidation process (becoming
rancid). The primary degree of this deterioration is the formation of hydro-peroxides
which attach them-selves to the carbon atom adjacent to the double bond:

H
|
R - CH = CH - CH 2 - R R - CH = CH - C - R
|
O - OH

The early part of the reaction (A – B) is autocatalytic and may be represented

graphically in Figure 1

Destruction of Peroxides
PV

B
Autocatalytic
oxidation
zone

A
Time

Figure 1: The Autocatalytic Oxidation Zone

Only the first part of the curve is representative of the degree of oxidation of the
material.

The determination of peroxide value has made it possible to study the stability
of palm oil in relation to oxidation. However, the correlation between peroxide value
and the degree of oxidation of the oil applies only in the early stage of oxidation

100
because peroxides are very unstable (decomposition accompanied by release of
energy).

Peroxide Value of Freshly Prepared Oil

All results are expressed as milli equivalents per kilogramme of the material. A
peroxide value of 1 corresponds to 0.008 g of oxygen per kg.

The determination procedure gives an accuracy of 0.5 peroxide value. It

should be noted that the Wheeler value is expressed as millimoles of peroxide per kg
(A wheeler value of 1 corresponds to 0.016 g of oxygen per kg of material).

Several other methods of assessing the oxidation status of oil have been tried,
among which only the thiobarbituric acid (TBA) method deserves further
consideration . The procedure is however difficult to use and less straightforward than
the iodometric method which is the popular method currently used by the industry.

The Pattern of oxidation as assessed by the determination of peroxide value

according to Wheeler is not identical to that obtained by the TBA method as shown
by the oxidation curves of oil in the course of time as illustrated in Figure 2.

FIGURE 2: OXIDATION AT 105 O C OF OIL AS MEASURED BY THE

PEROXIDE VALUE AND TBA VALUES (milliequivalent/kg)
PV & TBA (meq/kg)
40

35

30

25 Wheeler Peroxide Value

20

15 TBA Value

10

0
1 2 3 4 5
Time in hours

101
 Oil in the fresh fruit has a peroxide value lower than 1. After extraction under
favourable conditions, the peroxide value is lower than 2. After storage in the country
of production, handling and transport to Europe or America, the peroxide value ranges
between 1 and 12. Of the samples drawn ex ship’s tanks in the port of discharge, 81%
had a peroxide value of 5 or lower. No specifications as regards peroxide value of
palm oil have been published in the technical literature. However, Hadorn and
Jungkuntz recommend the following general specifications for oil:

Peroxide value between 0 & 3 = the oil can be stored.

Peroxide value between 3 & 6 = the oil can be stored for a limited period.
Peroxide value between 7 & 10 = the oil must be refined without delay.
An exception is made for olive oil for which a peroxide value of 8 to 10 is considered
normal.

The increase in peroxide value of oil in bulk of large tonnage is perceptible

only after several weeks of storage. Small amounts of oil, for which the ratio of
surface to volume is of consequence, show a sharper increase in peroxide value.
Table 2 shows the pattern of oxidation on samples of approximately 100 g stored in
250 ml beakers at ambient temperature. In order to shorten the time of recording, that
is to accelerate the oxidation process, a storage temperature of 60°C is normally used.
At the temperature, the oxidation process is about 8 times faster.

TABLE 1. PEROXIDE VALUE OF OIL STORED AT AMBIENT TEMPERATURE

Time (in days)

Type of oil
0 6 27 53 71
Crude oil obtained by centrifugal 0.7 1.1 1.0 1.9 2.0
extraction
Crude oil extracted by pressing 1.3 6.7 13.1 12.9 17.1
Water washed crude oil 1.1 2.1 4.3 3.0 4.2
Oil extracted with trichloroethylene 1.3 2.4 3.5 3.8 3.3
Oil extracted with xylene 1.1 1.9 2.3 2.1 3.0
Note: Crude oil extracted by pressing contains a large amount of water and impurities
and ferments during storage.

102
Factors Affecting Peroxide Value
Laboratory Tests
The following factors were studied:
• drying;
• heating under inert atmosphere;
• washing;
• de-gumming;
• carotene content; and
• initial peroxide value.
The experimental procedure consists in the determination at periodical
intervals of the peroxide value of oil stored at 60°C. In some series of experiments,
the samples were kept in darkness as carotene exerts a pro-oxidizing effect in the
presence of light and an anti-oxidizing influence in darkness. Numerous treatments
were applied. The conclusion was reached that they are very seldom beneficial to the
storage of oil and that in certain instances they are markedly deleterious. The
washing with surfactant for instance (quaternary ammonium and various alkyl-aryl -
sulphonates) is clearly unsuitable.

Only the storage in sealed tubes of oil with or without prior treatment leads to
a remarkable stability as regards peroxide value. A marked bleaching (destruction of
the carotene) is however apparent.

Table 2 gives a summary of the results obtained through the following

treatments”
• control;
• oil dried during 1 min at 110°C;
• oil stirred with water in a turbo mixer for 15 seconds at 50°C;
• oil stirred as in 3 but solution of A.A.S.* in a turbo mixer;
• oil treated as in 5 but subsequently dried.
* alkyl-aryl-sulphonate.

TABLE 2. PEROXIDE VALUE AND COLOUR OF TREATED OIL STORAGE AT 60°C

103
 Treatment
Day of storage 1 2 3 4 5 6
Initially 1.7 3.2 - 3.1 2.2 3.2
4 days (open container) 7.3 12.0 10.2 9.0 8.2
14 days (open container) 37.5 39.2 40.5 - 56.0 41.1
5 days in sealed container 1.1 1.1 1.4 67.8 1.0 1.2
Colour expressed as optical density
Initially 87 91 90 86 89 87
4 days 81 78 79 70 75 76
10 days 49 28 20 5 7 2.6

Washing with citric acid and sodium ethylene- diamine-tetracetate does not lead to
improved keep ability.

The drying of oil, its effect on peroxide value and on the ability to withstand storage
have been studied with the Swift apparatus using samples containing 0.3% moisture.
Air insufflation at 80 o C, 100 o C, 120 o C, & 140 o C was used.

In all cases air bubbling was continued until moisture content had been reduced to
O.05%. As shown in Table 72, the drying induces an increase in peroxide value but
very small maginitude.

Although peroxide value remains fairly steady during drying, it was necessary
however to ascertain whether the drying did not make the the oil susceptible to post
oxidation during subsequent storage, that is if oxidation did not become prevalent for
the treated samples. The storage of oil in thin layer in Petri dishes showed no
difference between the treated and untreated oil. On the contrary , the partial
oxidation sustained by oil during drying appears to slow down further oxidation to the
point that the untreated oil eventually “catches up” with the oxidized oil ( Table 4
(73))

104
 Table 3 : Evolution of Peroxide Value as a Result of Drying with Air

Time
80 o Celsius 100 o Celsius 120 o Celsius 140 o Celsius
% Peroxide % Peroxide % Peroxide % Peroxide
moisture value moisture value moisture value moisture value
Initial 0.30 3.5 0.30 3.5 0.30 3.5 0.30 3.5
30 sec - - - - - - 0.13 3.9
60 sec - - - - 0.09 4.0 0.08 4.0
2 min - - - - 0.04 4.2 - -
3 min - - - - 0.03 4.0 - -
4 min - - - - 0.01 4.5 - -
5 min 0.19 3.5 0.04 4.5 - - -
10 0.04 3.6 0.02 4.9 - - -
min
15 0.07 4.0 0.02 5.0 - - -
min
20 0.01 4.1 0.02 5.9 - - -
min

Table 4 Storage of dry oil at 60o C

Time lapse Initial oil Oil dried Oil dried Oil dried Oil dried
at 80 o C at 100 o C at 120 o C at 140 o C
Moisture content 0.30 0.03 0.05 0.05 0.06
Initial peroxide value 3.5 4.1 5.0 4.4 4.4
After 3 days 5.5 6.0 6.5 6.1 6.3
After 8 days 7.7 8.0 9.2 9.1 8.3
After 17 days 13.0 12.8 13.0 12.8 14.0

Similar experiments were carried out at various temperatures with identical results. It
may be concluded therefrom that the drying of oil by air bubbling, although
detrimental a priori, does not impair the quality of oil in the course of storage. The

105
point was important because a deterioration would have prevented the used of air
drying and would have made it mandatory to use vacuum drying for instance.

Absorption of Air
Whilst very little oxygen is taken up at low temperature during contact between oil
and air, a marked absorption of the latter takes place. The removal of air from oil at
high temperature enables the absorbed constituents to be titrated. The rate of
absorption can be measured in the Warburg apparatus. In the course of an ageing test
over 50 hr at 80°C, oil takes up a little more than 100% of its volume, therefore about
0.1% of its weight. Only a fraction of the oxygen of the absorbed air is combined in
the form of peroxide. Table 5 give values of the following against time: peroxide
value, volume of absorbed oxygen, the corresponding milliequivalent value of
oxygen per kg of oil and the ratio of combined to absorbed oxygen (temperature
80°C).

TABLE 5 ABSORPTION OF OXYGEN DURING STORAGE

Time Initial peroxide Peroxide Volume of oxygen Milliequivalents Ratio of fixed
(hr) value value absorbed per unit of absorbed to absorbed
increase volume oil oxygen oxygen
0 6.7 0 0 0 -
6 10.9 3.2 0.81 57.2 16%
21 – 14.5 7.8 0.96 79.0 18%
25
47 – 24.7 18.0 1.07 88.8 20%
49

De-gumming appears to intensify the increase of peroxide value during

storage. On the other hand oil containing added mucilages shows improved stability.

Heating in an inert atmosphere reduces the peroxide value of oil. From an

initial level of 8.5, peroxide value decreases to 5.6 after 30 min of heating at 115°C
and 1.3 if 130°C is used. A portion of carotene is destroyed by the treatment (10% to
12%).

The effect of iron, whether in the form of metal or of soap is hardly noticeable
or non-existent.

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 The initial peroxide value governs the pattern of the oxidation curve. The fact
has been observed on sample of oil of vary different peroxide values as has been
recorded in technical publications. The results of a few observations made on
samples of oil with low peroxide value are collected in Table 6.

TABLE 6 : EVOLUTION OF PEROXIDE VALUE AS A FUNCTION OF THE

INITIAL PEROXIDE VALUE

Initial After After After % Mg of carotene for 100g of

P.V. 4 days 8 days 17 days F.F.A oil
0.3 0.9 1.5 5.8 1.1 34.6
0.5 0.9 2.3 5.0 2.6 40.1
3.6 9.1 12.7 13.4 5.1 65.5
4.2 11.6 14.0 10.4 1.3 37.6
4.8 10.9 14.8 16.1 1.3 39.4
5.1 13.2 19.2 21.5 1.0 61.8

Industrial Trials
The washing of oil with detergents has been used extensively. This technique
had been adopted as a result of the beneficial affect reported by users, particularly in
the U.S.A. Following a large number of shipments of Congo oil to Europe and the
U.S.A., tt has been possible to establish that the use of detergents made the oil
sensitive to oxidation. No difference in peroxide value is detectable immediately
after the treatment but after a few weeks, the oxidation of oil increases sharply then
seems to tend towards limit of 12 to 15. The washing of oil with detergents has
consequently been stopped in Africa but still prevails in the U.S.A for oil used in
metallurgy.

Nature of the Peroxides of Palm Oil

Because the study required complex techniques it was not our intention to investigate
the composition of the peroxides formed in the course of storage. We proposed
however, to find out whether the peroxides of palm oil were peroxides of the
unsaturated fatty acids or carotene. With this objective in view, the peroxides were

107
isolated by chromatography. The technique was tested on ground nut oil that applied
to palm oil.

The use of a solution of oil in chloroform on a Brockmann alumina column

and elution with chloroform lead to no retention of peroxide and hardly any of colored
substances. On the other hand, when a solution in petroleum ether is used the
peroxide value of the elute is nil and various coloured bands appear. Elution with
chloroform, after drying under nitrogen, of these coloured bands leads to the
observation that none of these bands has a special status as regards peroxide retention.
The distribution appears to be uniform.
The use of Filtrol instead of alumina leads to marked retention with petroleum
ether solution and elution with chloroform. The retention is less intense for the
chloroformic solution and elution by the same solvent.

In order to separate the carotenes from the peroxides, use has been therefore
made of the petroleum ether solution, which removed the corotenoids leaving the
peroxides, the latter being recovered by successive elutions with chloroform.
Table 7 gives the results of the technique applied to palm oil with a peroxide
value of 24.7 and ground nut oil with a peroxide value of 21.8.

TABLE 7 . PEROXIDE VALUE OF DIFFERENT FRACTIONS

Petroleum ether Chloroform

1 2 3 4 5 Total
Palm oil 0 20.2 0.7 3.2 0.7 25.5
Ground nut oil 0 16.9 3.2 1.2 1.0 22.4

In the case of palm oil, the carotenoid bands are practically eliminated by the
petroleum ether. In the case of ground nut oil, the yellow band is eluted in the 3 rd
fraction. The carotenoid content of the various fractions was determined through
measurement of the optical density.
Table 8 gives the results of this test and Figure 2 gives the spectrum of the first four
fractions.
TABLE 8 . PEROXIDE VALU AND OPTICAL DENSITY OF VARIOUS FRACTIONS

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 Type of solvent Petroleum ether CHCL3
Fraction of solvent 1 2 3 4 5 6 7
Peroxide value 0 5.7 5.1 2.3 2.3 5.2 0.6
Optical density at 420 mµ 16.5 10.2 01.5 0.4 1.7 5.2 0.6

Figure 3. Absorption Spectrum of Fractions of Palm Oil of 24.7 Peroxide Value

obtained by Chromotography on Brockmann Alumina using Petroleum ether as
Eluting Medium.

It may be concluded that although the elution of peroxides overlaps that of the
various colored bands of the oil, it is however, possible to modify these overlaps by
suitable selection of the eluting solvents. There existing, therefore, a strong
probability that peroxide which do not given the typical spectrophotometric curve are
not proxides of carotenoids.

109
 The similarity between the results obtained for palm oil ground nut oil
respectively makes it possible to identical in both cases. This leads to the conclusion
that the peroxides of palm oil are indeed derives from fatty acids and not from
carotene.

110