Journal of Oil Palm Research Vol. 12 No. 1, June 2000, p. 107.

116

SURFACE he supernatant sludge from the palm

oil mill was determined to be surface

ACTIVE active from surface tension measure-

ment. In crude palm oil (CPO)lsludge super-
PROPERTIES natant, the inter-facial tension was determined

OF PALM OIL to be 3 mN m-r which is fauourable for the

formation of oil droplets in the CPO slurry.
WITH RESPECT The refined oillwater systems have higher
interfacial tension compared to the CPOlwater
TO THE system. Depending on whether the CPO is chemi-

PROCESSING cally or physically refined, the oil/water inter-

facial tension differs and can be as high as 25.6
OF PALM OIL mN m-l and 12.7 mN rn~r respectively compared
to an interfacial tension of 8.00 mN m-r in the
CPOlwater system. The higher inter-facial ten-
sion value indicates more efficient removal of
surface active compounds from the chemically
refined oil. This may have great implications in
the quality and utilization of palm oil in food
Keywords: Interfacial tension, processing.
surface tension, surface active, sludge, crude
palm oil, refined oil, milling, refining. The interfacial tension values of the partially
refined oils as sampled from various points of
refining were found to increase as the oil is
processed. In uiew of this increase, interfacial
tension could possibly be used as a process

CHOW, M C* and HO, C C** control parameter in the refining of CPO.

Lecithin and monoglycerides were deter-
mined to significantly reduce the interfacial
te’nsion at the refined palm oil lwater interface.
Some of the common minor constituents found
in CPO such as carotene, diglycerides, fatty acids
* Malaysian Palm Oil Board,
P.O. Box 10620, 50720 Kuala Lumpur, Malaysia. and cholesterol did not show surface activity at
** Chemistry Department, Universiti Malaya, Lembah Pant& 50603
Kuala Lumpur, Malaysia. the refined palm oillwater interface.

107
JOURNAL OFOIL PALM RESEARCH 12(l)

INTRODUCTION required throughout the milling process. Hot

water is further added to the crude oil slurry to

P alm fruits are harvested in bunches and

sent to the mill for processing (Figure I).
On arrival, the bunches are steam sterilized
reduce the viscosity so that the oil will cream to
the surface in large clarification tanks. The
underflow from the lower section of the clarifi-
where the fruits soften and are easily detached cation tank is centrifuged to remove as much of
from the stalk. These detached fruits are further the heavier phase consisting of solids and water.
softened with steam in digesters. The digester This watery phase or sludge is discharged and
mash is then passed to the screw press where oil any oil found here constitutes oil loss as it is
together with the juice from the fruits are discharged as effluent, The lighter phase from
expressed. The crude oil slurry which is ex- the centrifuge, which consists of oil and water,
pressed may contain approximately 48% oil, is recycled to the clarification tank. The creamed
45% water and 7% solids. Some of the water in palm oil from the surface of the clarification
this slurry is actually steam condensate from tank is then skimmed and further purified,
the sterilization, digestion and screw pressing dried and sold as CPO to the refinery for further
where steam is injected into the respective processing.
machinery to maintain the high temperature

Fresh fruit bunches.

piiq . Condensate effluent

b Empty bunches

Fibres and nuts to

* kernel plant for
kernel separation
Water addition

Light phase

.
SLUDGE
Effluent

Figure 1. Flow diagram of palm oil extraction.

108
 SURFACE ACTIVE PROPERTIES OF PALM OIL WITH RESPECT TO THE PROCESSING OF PALM OIL

In the refinery, the CPO is processed to They are free fatty acid, moisture and impuri-
remove most of the undesirable impurities thus ties, and, in some mills, the peroxide value,
making the oil bland, colourless and chemically which determines the degree of oxidation.
stable according to trade specifications and Similarly, in the trading of refined palm oil,
consumer requirements, There are basically two the same set of contractual specifications are
types of refining practiced by the Malaysian required with the additional requirement of
palm oil refiners. They are chemical and physi- colour. These parameters are used to assess not
cal refining. The two processes differ in treat- only the initial quality of CPO but also the
ment of the oil and result in differently labelled amount of bleaching earth required which is one
oils as illustrated in Figure 2. of the major costs incurred in CPO relining. No
In the mill, as the CPO is extracted there form of continuous monitoring is known in palm
is no continuous on-line monitoring of quality oil relining.
but the impurities present are only of botanical This study reports an alternative qualitative
origin from,the palm fruits. In the final quality parameter, interfacial tension, which can pos-
assessment when sold to the refineries, only sibly be used to assess the effectiveness of each
certain contractual specifications are measured. stage of the refining process. The significance

*Crude palm oil “Crude palm oil

Ortho phosphoric Ortho phosphoric

acid acid
I I
Degummed oil Degummed oil

Caustic soda Bleaching earth

I I
‘Degummed and “Degummed and
neutralized oil bleached oil

Water washed
Steam deodorization
and vacuum dried
I I
Neutralized oil (NPO) ‘Refined bleached and
deodorized palm oil (RBDPO)
Bleaching earth
I
‘Degummed, neutralized and
bleached oil

Steam deodorization
I
‘Neutralized bleached deodorized palm oil (NBDPO)
Notes: * Samples of partially processed oil.
Adapted from Selected Readings on Palm OiZ and its Uses. Ministry of Primary Industries,
Malaysia, 1993, p. 150-174.

Figure 2. Refining processes for CPO.

109
JOURNAL OF OIL PALM RESEARCH 12(l)

and importance of this parameter in causing oil TABLE lb. QUALITY OF NBDPO
loss in the milling process is also discussed.
Free fatty acid
(as palmitic acid) 0.02%
MATERIALS AND METHODS Peroxide value 2.41 meq kg-’

Materials 4: 1.55

Sludge from the centrifuge of a palm oil mill 0.36

k,“,
was collected and analysed the following day.
High speed centrifugation at 10 000 G was used carotene 1 pm
to separate the suspended solids and the oil Anisidine value 1.31
droplets in which a clear brown supernatant
was obtained. This sludge supernatant was used
in subsequent interfacial tension and surface Methods
tension measurements.
CPO was collected from various palm oil The Kruss Digital Tensiometer Model KT 10
mills in Peninsular Malaysia. Some samples of was used for the measurement of surface tension
CPO and partially processed palm oils were and interfacial tension in the systems studied.
obtained from various refineries in Peninsular All water and oil samples were placed in a 60°C
Malaysia too. Commercial monoglyceride, PVP, oven before transferring to the tensiometer for
consisting of 90% monopalmitin and 10% measurement. All measurements were also car-
monoolein of 90% purity, was supplied by ried out at 60°C.
Grindsted Products A/S, Denmark. The lecithin
was type IV-S: (soyabean lecithin containing Surface tension measurement. The tensio-
approximately 40% phosphatidylcholine) sup- meter with the attached ring in air was tared.
plied by Sigma Chemical Co. Diglycerides of The sample was then brought up until the ring
dipalmitin and diolein, fatty acids palmitic and was submerged. The system was allowed to
stearic and cholesterol palmitate were also stabilize for half an hour and measurement
supplied by Sigma Chemical Co. Carotene con- began by slowly lowering the sample stage. The
centrate was an extract from CPO. ring pulled a collar of liquid into the air. The
Commercial chemical refined palm oil maximum force necessary to break the film in
(NBDPO) was used as the standard palm oil in air was taken as the surface tension of the liquid.
which other components were added in all the The ring was cleaned with methanol, acetone
interfacial tension measurements. The NBDPO and finally flamed after every measurement
used contained 95.97% triglycerides, 3.99% before the next.
diglycerides and 0.04% monoglycerides. The
fatty acid composition and some quality para- Interfacial tension measurement. The
meters are as shown in Tables la and b. tensiometer was tared in the lighter phase (oil)
by submerging the ring completely in it. Zero
adjustment in the oil was necessary to compen-
TABLE la. FATTY ACID COMPOSITION sate for buoyancy and surface tension which
OF NBDPO acted on the shaft of the ring. The ring was
Fatty Acid wt. (o/o) cleaned as described above.
After that, a new sample container was half
12:o 0.2 klled with the heavy phase (water, 12.5 g) and
14:o 1.0 the cleaned ring submerged into it. The lighter
16:0 43.9 phase (oil, 12.5 g) was added carefully to the
18:0 4.0 top of the water. The system was allowed to
18:l 40.6 stabilize for half an hour before the ring was
132 9.6 pulled through the oil/water interface. The
18:3 0.3 maximum force necessary to break the film in

110
 SURFACE ACTIVE PROPERTIES OF PALM OIL WITH RESPECT TO THE PROCESSING OF PALM OIL

the oil was taken as the interfacial tension of contains only botanical residues from the meso-
the system. carp or fleshy part of the fruit. It is not possible
The mean interfacial tension of the NBDPO to measure the surface tension in the presence
against water was 20.6 mN m-l at 60°C based of solids and thus the sludge had to be centri-
on measurements of 10 samples of the same fuged. On centrifugation, a clear brown
batch of oil. The measured values ranged from supernatant was obtained while the solids set-
19.2 to 21.6 mN m-l with a standard deviation tled to the bottom and the oil droplets which
of 0.72 mN m-l. creamed were separated. The supernatant ob-
tained from sludge was determined to have a
surface tension of 30 mN m-’ at 60°C compared
RESULTS AND DISCUSSION to water which has a surface tension of 66
mN m-l indicating the presence of surface active
Surface Activity agents in the sludge.
The surface activity ofthe sludge supernatant
Surface activity is manifested by groups of decreased linearly when plotted against the
compounds called surface active agents or logarithmic concentration of sludge diluted with
surfactants, commonly known as emulsifiers in water (Figure 3). However, at the same concen-
foods. The structures of these molecules are
such that they consist of two moieties; a hydro-
phobic chain linked to a hydrophilic functional -I

group. In view of the amphiphilic nature of the

emulsifiers irrespective of the phase in which
they are dispersed, they will tend to become
located at the interface be it the air/water, air/
oil or water/oil interface. The hydrophilic head-
group will tend to locate itself in the aqueous
phase while the lipophilic hydrocarbon chain
orientates towards the oil phase, this situation
being thermodynamically more favourable than
complete dissolution in any particular phase.
This phenomenon of lowering the energy level
at the interface between the two phases is
measurable and is termed surface tension ifone
of the phases is air while that which occurs at
two liquid phases such as oil/water is termed
interfacial tension. Through such determina-
tion, the surface activity caused by the presence
of the surface active compounds can be detected
and determined by a surface tensiometer. Fur-
ther lowering of the energy at the interface will
result in a lowering of the surface or interfacial
tension which will be conducive for emulsifica-
tion or droplet formation when mixing. At
extremely low interfacial tension, spontaneous
0-l
emulsification will result in the formation of q
microemulsions and when the interfacial ten- 0.1 1 10 100
sion is negligible complete miscibility or disso- Wt. % sludge supernatant in water
lution of the two phases takes place.
Figure 3. Effect of dilution with water at 60°C on the
Milling surface tension of sludge supernatant and interfacial
tension of palm oil (NBDPO) and CPOlsludge
In the mill, the liquid discharged (sludge) supernatant interface.

111
JOURNAL OF OIL PALM HESEARCH 12(l)

tration of sludge supernatant in water when cess (Yamaoka et aZ.,19891. These molecules can
different types of palm oil was present at the act as natural biosurfactants in the GPO/sludge
interface, there was a further reduction in the supernatant interface and further stabilize the
interfacial tension but the decrease was not as droplet surface as even when these droplets
sharp when compared to the surface tension of from the sludge are concentrated they do not
the supernatant only (Figure 31. coalesce easily to form a homogenous layer.
The reduction of interfacial tension of the Evidence ofsurface active agents in the CPO
NBDPO/sludge supernatant system compared is further illustrated in the decrease of inter-
to the surface tension of sludge supernatant facial tension at the NBDPO/water system
at the same concentration indicated that the (Figure 4) when CPO is added to the NBDPO
oil/supernatant system had a lower free energy which is a relatively purified commercial palm
than the supernatant/air system. This could oil. Other known commercial vegetable oils such
possibly be due to more favourable orientation as olive, corn, canola and olive oils have inter-
of surface active agents from the supernatant facial tension ranging from 19.0-23.0 mN m-l
preferentially absorbed by the oil phase. How- and when purified through Florisil had their
ever, the interfacial tension of the GPO/sludge interfacial tension increased to 30532.0 mN
supernatant was further depressed compared to m-l (Goankar, 1989).
the NBDPO/sludge supernatant system. This
could possibly indicate that there were also
surface active agents in the CPO. In the undi-
luted sludge supernatanffCP0 system, the in-
terfacial tension was reduced to 3 mN m-l which
was sufficiently low for emulsification to occur.
The GPO/sludge supernatant system is a
close simulation ofthe clarification station ofthe
milling process where there is intimate contact
of the two liquid phases. Together with the
intensive agitation of pumping and high tem-
perature, the conditions are ideal for undesir-
able emulsion formation. Optical microscopy
showed that these oil droplets are indeed present
in sludge (Chow, 1987). As much as 30% of the
total oil found in the sludge is actually in the
form of minute droplets.
In emulsification, once the droplets are
formed, subsequent stabilization of the oil drop-
lets must occur otherwise the droplets may
rapidly flocculate and coalesce separating into
the respective original phases. The stability of
these newly formed droplet interface may depend
on the interaction of the various surface forces
of the molecules at the interface (Bergenstahl
and Claesson, 1990). Mixed emulsifiers at the
surface of the droplets may form stable com- 0 20 40 60 80 100
plexes which stabilize the droplets (Boyd et al.,
1972). Monoglycerides, diglycerides, glycolipids Concentration of CPO added to NBDPO
and phospholipids are natural. biosurfactants (wt. %)
and are known to be present in CPO (Gob and
Timms, 1985; Kulkarni,l991;Goh et c&19821.
Glycolipids at as high as 3.8% are found in oil Figure 4. The effect of CPO on the interfacial tension
from spent earth discarded in the refining pro- of NBDPOlwater interface.

112
 SURFACE ACTIVE PROPERTIES OF PALM OIL WITH RESPECT TO THE PROCESSING OF PALM OIL

Refining higher interfacial tension ranging from 25.0 to

26.4 mN m-i compared to physically refined oil
The surface tensions of various commercial with interfacial tension ranging from 10.6 to
palm oil products had been measured previously 12.9 mN m-l (Table 2) indicating that chemical
at specific temperatures but no significant refining was capable of removing more impu-
variations were found (Oh and Chong, 19921. rities that were surface active. The presence of
The present study also showed that at 6O”C, the such substances in the oil may have great
surface tension of palm oil at .various stages of implications in the quality and utilization of
refining were very similar within a narrow palm oil in food manufacturing.
range of 30.6-31.7 mN m-l but that their inter- Surface active agents in palm oil may in-
facial tensions varied and decreased differently clude monoglycerides, glycolipids and phospho-
as the oil was processed (Table 2). The presence lipids. Hydrolysis products such as fatty acids,
of surface active agents in CPO and its products aldehydes, ketones, hydroperoxides and pero-
was clearly manifested in their low and varied xides are some of the impurities removed in the
interfacial tension values but not in the surface refining process. Carotene breakdown products
tension values. This also indicated that the are also subsequently removed in the refining
surface active compounds present in the oil process. These minor by-products could possibly
were thermodynamically more favourably ab- play a role in affecting the properties of the bulk
sorbed at the oil/water interface than at the phases and thus affect the interfacial property.
oil/air interface. The surface active agents present At each stage ofdegumming, neutralization and
in the oil had greater affinity for water or are bleaching of the oil, more surface active sub-
relatively polar. stances are removed as shown graphically
The interfacial tension of GPO/water inter- (Figure 5) by the increase in interfacial tension
face ranged from 6.0-9.6 mN rn~l. As the oil is of the oil against water. In chemical refining,
processed, the interfacial tension is increased. the degumming and neutralization seemed much
Chemically refined oils were determined to have more effective than bleaching in the removal of

TABLE 2. SURFACE TENSION OF PALM OIL AND INTERFACIAL TENSION OF

PALM OIL/WATER INTERFACE AT VARIOUS STAGES OF REFINING MEASURED AT 60°C
Oil* Interfacial tension Surface tension
against water bN m-9 (mN m-1)
Range Mean S.D. Range Mean S.D.
=Crude palm oil 6.0- 9.6 8.0 1.2 30.6-30.9 30.8 0.1
b Degmmned and bleached
palm oil 10.1-15.6 11.8 1.7 30.8-31.0 30.9 0.1
b Refined, bleached and
deodorized palm oil (RBDPO) 10.6-12.9 12.7 1.1 30.8-31.1 30.9 0.1
= Degummed and neutralized
palm oil 18.9-24.2 20.8 1.8 31.0-31.7 31.2 0.1
c Degummed, neutralized and
bleached 24.7-25.4 25.0 0.3 30.7-31.0 31.0 0.1
r Neutralized, bleached and
deodorized palm oil (NBDPO) 25.0-26.4 25.6 0.5 30.8-31.1 31.0 0.1

Notes: aBased on 18 samples.

bBased on 11 samples (physical refining from four refmeries).
<Based on seven samples (chemical refining from two refineries).
Five hourly samples from one refinery and another two from another refinery.
*Point of sampling. Refer to Figure 2.

113
JOURNAL OF OIL PALM RESEARCH 12(l)

refineries. This low standard deviation of the

interfacial values could possibly be because a
rather limited number of samples (from only
two refineries) were analysed. Only five hourly
samples were collected from one refinery and
another two from the second refinery as chemi-
cal refining was usually carried out infrequently
and increasing the samples size during the
study was not possible.
Finally, deodorization at high temperature
has a strong influence on the amount of volatile
impurities removed but not so much on the
removal of the associated surface active com-
pounds, since the interfacial tension was not
significantly changed in both the physically and
chemically refined oils before and after the
deodorization process. In chemically refined oil,

I
Crude
palm
Degummed &
‘neutralized
Degummed
“neutralized
Refined
‘neutralized
deodorization only increased the interfacial
tension by 0.6 mN m-l from 25.0 to 25.6 mN
ml. In physical refining after deodorization, the
interfacial tension increased by 0.9 mN m-i
from a mean of 11.8 to 12.7 mN m-l.

oil & bleached bleached & Effect of Additives

deodorized

Note: *Neutralization is only carried out in chemical Since the interfacial tensions ofthe CPO and
refining. NBDPO are so different, an attempt was made
to study this parameter by individually adding
Figure 5. Changes in interfacial tension at the palm to NBDPO some common constituents that are
oil/water interface as the oil is chemically Iphysically known to be present in CPO. These include fatty
refined. acids, carotene, cholesterol, phospholipids and
partial glycerides of mono and diglycerides.
surface active substances from the oil as the The effects of various additives on the in-
changes in interfacial tension increased from a terfacial tension of the NBDPO/water system
mean of 8.00 to 20.8 mN m-* (difference of 12.8 are shown in Figure 6. Palmitic and stearic acid
mN m-l) after degumming and neutralization changed the interfacial tension only marginally
while there was an increment from 20.8 to 25.0 even when as high as 5% w/w was added sepa-
mN m-l (difference of 4.2 mN m-l) after bleach- rately to the refined oil. In fact, the interfacial
ing. Variation in the interfacial tension of the tension was increased slightly with the addition
bleached oil may depend not only on the prior of palmitic acid. A very slight reduction in
process of degumming and neutralization but interfacial tension was observed when choles-
may also be dependent on the type (surface terol was added to the oil. Similar findings were
activity) and dosage of bleaching earth used as reported by Ogino and Onishi (1981) on oleic
well as the duration and temperature of the acid and cholesterol which were shown to have
respective treatment Wrishnan, 19831. A larger insignificant effect on the corn oil/water inter-
variation in the interfacial value of bleached oil face. Carotenes up to as high as 10 000 ppm
is expected ( compared to a standard deviation added to NBDPO did not have any effect on the
* 0.3 mN m-l obtained) if samples from more interfacial tension of the NBDPO/water system.
refineries could be obtained. A higher standard Neither did diglycerides of dipalmitin or diolein
deviation of il.7 mN m-l was obtained in the at as high as 3% w/w affect the interfacial
bleached oil samples from the four physical tension of the NBDPO/water interface.
 SURFACE ACTIVE PROPERTIES OF PALM OIL WITH RESPECT TO THE PROCESSING OF PALM OIL

and Timms, 19851 and thus, most probably,

monoglyceride is the surface active agent re-
moved as the oil is refined whereby interfacial
tension of the NBDPO/water system is raised.
Various extent of lowering the interfacial ten-
sion of purified corn oil/water interface by
mixtures of monoglycerides has also been re-
ported (Goankar, 1989).
When soya lecithin was added to the NBDPO,
there was a rapid decrease in interfacial tension
at the oil/water interface (Figure 6). At 0.25%
w/w, the interfacial tension was reduced to
about 5 mN rn~l. At the same concentration of
lecithin or monoglycerides in NBDPO, the de-
crease in interfacial tension at the oil/water
interface caused by lecithin was much greater
compared to the monoglycerides. However,
phospholipids are only present in the range of
20-80 ppm in CPO (Gob et al., 1982). Although
phospholipids are more surface active compared
to monoglycerides, they probably are not as
significant as monoglycerides in increasing the
interfacial tension as the CPO was refined.
Phospholipids and monoglycerides may have
synergistic effect in reducing the interfacial
0.001 0.01 0.1 1 10 100
tension of the palm oil/water system. In view
of the phospholipids being so low in concentra-
Cow additives added to NBDPO tion in the CPO, its removal from the oil could
(wt. %) not have increased the interfacial tension as
significantly as the monoglycerides. Similarly
0 Palmitic acid + Stearic acid X Dipalmitin lecithin has been found to be surface active in
0 Diolein X Cholesterol A Palm oil carotene corn oil and safflower oil/water system too. At
0 PVP A Lecithin a concentration of 0.1% w/w lecithin in the oil,
the interfacial tension was reduced to as low as
Figure 6. Effect of various additives on the interfacial about 2 mN m-i (Ogino and Onishi, 1981).
tension of NBDPOlwater interface.

CONCLUSION
When commercial monoglycerides PVP, a
mixture of 90% monopalmitin and 10% mono- The aqueous supernatant from the palm oil mill
olein, was added to NBDPO, the decrease in sludge was determined to be surface active and
interfacial tension at the NBDPO/water inter- to have a synergistic effect in lowering the
face was gradual up to 0.2% w/w (Figure 6). interfacial tension of a GPO/water system. This
Above 0.2% w/w, a rapid decrease in interfacial resulted in the formation of undesirable stable
tension with PVP concentration was noted. The oil droplets in the sludge discharge. Further
interfacial tension was reduced from 19 to about studies had been carried out to determine the
6.5 mN mu’ at 1.25% w/w PVP. The NBDPO used quantity of such surface active agents that
contained 0.04% monoglycerides and additional contribute to the surface activity at the palm
monoglycerides further decreased the interfa- oil/water interface (Chow, 1997).
cial tension. CPO is known to have a monogly- Under current practice, refining of palm oil
ceride content ranging from 0.26%-0.31% (Gob is not intensively monitored except for colour

115
JOURNAL OF OIL PALM RESEARCH 12111

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116