SUMMARY

An Experiment was conducted to study and analyze the Dry Fractionation of

Refining, Degumming, Deodorising Palm Oil (RBD Oil). Dry Fractionation is a separation
process for oils. In this case, RBD oil was used and separated into two fractions, Olein and
Stearin. This separation process involved two section which is Crystallization section and
Filtration section. In Crystallization process, the RBD oil was feeded and heated to around
80°C - 85°C using the hot water system. The heated oil was then cooled in a controlled
environment to form crystals degree by degree. Cooling system sequences follows a
defined program using programmable controller. The lowering of temperature causing oil
with higher melting point to separate from the solution. The slurry of crystals and oil is then
pumped to the Filteration Section to proceed with the separation of solid crystals (Stearin)
from the oil (Olein). In Filtration process, an automated membrane filter press was used.
Stearin crystals will remain remained while olein passes through the filter. Based on the
result, production yield RBD palm oil feed to RBD palm oil Olein is 50.0%. The
experiment proceeded with the analysis of iodine value of feed RBD oil and both olein and
stearin from the result which was calculated 51.18, 57.95 and 46.74 respectively.
INTRODUCTION
Dry Fractionation is a process to separate vegetable oils such as palm oil into two
fractions which are Olein and Stearin by the crystallization properties of the oils.
Fractionation process is defined as a natural and value adding physical oil modification
process which creating no undesirable by-products (Harris, n.d.). Fractionation process is
also a process where it consists of a controlled cooling of the oil which is then producing a
partial, or ‘fractional’ crystallization (Calliauw & Ballestra, 2019).

Dry fractionation of fats and oils is the simplest and the cheapest among fractional
crystallization processes. The dry fractionation process mainly consists of two steps which
typical consists of Crystallization Section and Filtration Section (“Dry Fractionation Plant,”
2019). The first step is the crystallization process which the solid crystals are produced in a
liquid matrix by a cooling process. The product of stearin and olein were form after the
crystallization process.

The crystallization process is carried out in order to remove the higher melting
glycerides which can cause the liquid oils to become cloudy and more viscous at low
temperature. There are 3 factors which are temperature, time and agitation that will affect
the formation and character of the crystal. The importance of the factors are to reduce the
temperature due to the supersaturating the higher melting component which to separate
from a solution, the agitation which facilitates the formation of small crystals and the time
with a gradual decrease in temperature which promotes the formation of longer crystals.
The crystallization system is a batch type and is equipped with special crystallizers
operating alternatively.

The second step is a filtration process where the liquid phase is separated from the
crystals. Filter press is considered more economical by many users of fractionation plants.
The advantage lies mainly for the higher olein yield by applying a pressure to the cake
during filtration. High pressure can expel the liquid fraction that physically trapped on the
crystal (Nusantoro, 2007). The olein quality is normally not affected by the filtration
pressure unless stearin passes through the filter cloth.

In contrast to the other fractionation process such as detergent or solvent

fractionation, dry fractionation does not require any additional substances. The results
collected from the dry fractionation are stearin which is a hard-fraction and olein which is a
liquid-fraction. The dry fractionation process was done in a pilot plant crystallizer equipped
with high pressure filtration. It has been done an investigation about dry fractionation of
RBD-palm oil to obtain stearin and olein fractions.

The goal of fractionation process is to create the biggest possible difference between
two fractions (Nusantoro, 2007). Palm oil is by far the most fractionated oil in the world.
The olein fractions are used as a substitute for soft oils in frying, cooking and salad oils or
are being further fractionated. The major advantage of palm olein is its high stability during
frying that produced minimum amount of breakdown products in an acceptable level.
However, palm olein tends to crystallize at low temperature that limits its usage in
temperate countries. . Palm olein has been chosen as the feedstock due to its higher
unsaturation content compared to palm oil.
METHODOLOGY

Plant operation

1. The RBD palm oil with (IV value range of 50-55) was preheated to 45°C in storage
tank T704.
2. The chilled water tank was filled with tap water and the packaged chiller unit was
switched on to produce chilled water at about 10°C.
3. The hot water tank TI13 was filled with tap water and electrical heating element
HT113 was switched on to produce hot water at about 90°C. The water temperature
was set at temperature controller TIC113.
4. The cooling program for crystallizer TI11was set at temperature controller TIC111.
5. Pump P704 was started and the oil from the storage tank was fed to crystallizer
TI11. At high level HLAII1, pump P704 was stopped and mixer AG 111 was
started. The frequency inverter was used to adjust the mixer speed.
6. Pump PIIO was started and the water temperature was set to 80-85°C at temperature
controller TIC 111.
7. Pump P113 was started and hot water from hot water tank TI13 was fed to the
cooling coil of crystallizer TI11 to heat the oil to 70°C.
8. Pump was switched to chilled water tank and chilled water was fed to the cooling
coil of crystallizer TI11 to cool the oil according to the program.
9. Filter FI11 was closed and pump PI11 was started and the oil was filtered through
filter FI11. The liquid fraction (olein) were flowed into olein tank TI14 while solid
fraction (stearin) was formed a cake in filter chambers.
10. Pump PI11 was stopped and the stearin cakes were squeezed by feeding compressed
air. The trapped olein in the stearin cakes were squeezed out.
11. The stearin cakes were removed from the filter chambers and dropped into stearin
tank T115. Steam was flowed to the internal heating coil of the stearin tank to melt
the cakes.
 12. When crystallizer TI11 was emptied, mixer AG111, pump PIIO and pump P113
were stopped. The packaged chiller unit and electrical heating element HTI13 were
switched off. The temperature controller was stopped.
13. Pump PI14 was started and the oil was transferred in olein tank TI14 for next
processing stage. Pump PI14 was stopped when olein tank was empty.
14. The drain valve of stearin tank TI15 was opened and the oil was transferred to next
processing stage. Steam flow was stopped.
15. The sample was ready to analyse.

Analysis procedure

1. The sample was melted and any solid impurities were removed and filtered.
2. After filtration, the sample allowed to achieve a temperature of 68°C-71°C before
weighing the sample.
3. The sample was weighed into a 500ml flask.
4. The different volume of solvent was added on top of the sample and the sample was
swirled to ensure it completely dissolved.
5. 25ml of Wijs reagent was added using the pipette into the flask containing the
sample. Using a stopper, the flask was swirled to ensure an intimate mixture.
6. A blank with solvent and reagent was prepared.
7. The flasks were stored in the dark room for 1 hour at temperature of 25°C.
8. The flasks were removed from the storage and 20 ml of potassium iodide (KI) was
added followed by 150ml of distilled water.
9. The solution was titrated with standard sodium thiosulphate solution until the
yellow colour disappeared.
10. A few drops of starch indicator solution were added and the titration was continued
until the blue colour disappeared after very vigorous shaking.
11. At least one blank was prepared with each group of samples.
12. The samples were analysed for each 30 min running hours of fractionation plant.
TABLE OF DATA
Table 1: Data of Experiment

Segment 1 Segment 2 Segment 3

Starting set point 60°C 40°C 30°C
(SSPI) in ℃
Target set point 40°C 30°C 22°C
(TSPI) in ℃
Time in minutes 163.1 mins 216.5 mins 154.8 mins

Temperature Vs Time
70

60

50
TEMPERATURE

40

30

20

10

0
0 50 100 150 200 250 300 350 400 450
TIME

Figure 1: Fractionation process on 3 segments

Weight of RBD Palm Oil feed: 8.0 kg

Weight of RBD Palm Olein: 4.0 kg

Production Yield = 50.0 %

Iodine value analysis

Table 2: Result of Iodine value for RBD Palm Oil feed

RBD Palm Volume of sodium Volume of sodium Mass of Iodine

Oil Feed thiosulphate solution thiosulphate solution test value
used for blank sample, used for the sample, M
V1 (ml) determination, V2 (ml) (g)
Sample 1 43.3 34.5 0.2 55.84
Sample 2 43.3 36.4 0.2 43.78
Sample 3 43.3 34.8 0.2 53.93
Average 51.18

Table 3: Result of Iodine value for RBD Palm Olein

RBD Palm Volume of sodium Volume of sodium Mass of Iodine

Olein thiosulphate solution thiosulphate solution test value
used for blank sample, used for the sample, M
V1 (ml) determination, V2 (ml) (g)
Sample 1 43.3 34.2 0.2 57.74
Sample 2 43.3 33.6 0.2 61.55
Sample 3 43.3 34.7 0.2 54.57
Average 57.95

Table 4: Result of Iodine value for RBD Palm Oil Stearin

RBD Palm Volume of sodium Volume of sodium Mass of Iodine

Stearin thiosulphate solution thiosulphate solution test value
used for blank used for the sample, M
sample, V1 (ml) determination, V2 (ml) (g)
Sample 1 43.3 36.8 0.2 41.24
Sample 2 43.3 35.2 0.2 51.39
Sample 3 43.3 35.8 0.2 47.59
Average 46.74
DISCUSSION
The main objective of this experiment is to perform separation of palm olein and
palm stearin from RBD palm oil via dry fractionation. A fractionation process consists of
controlled cooling of the oil, thereby inducing a fractional crystallization then the RBDPO
was separated to remaining liquid (palm olein) and solid fraction (stearin) by physical
treatment. In principle, dry fractionation was able to give good fractionation ads solvent
fractionation because the separation of triglycerides is independent of the solvent
(Timms,2005). Crystallization is an important step in dry fractionation. Crystallization is
when solid crystal was produced in liquid mixture during cooling process. Crystallization
during fractionation process can be categorize into two steps which are nucleation and
crystal growth. Nucleation is the ignition process that occurs in the formation of a crystal
from a solution in a low temperature (Hosch, n.d).

Based on result graph 1, there are three segments involved in the process of
fractionation. In the first segment, the segmented time to reach the target set point (TSPI) at
40℃ was 163.1 minutes. The second segment started at 40℃ to 30℃ in segmented time
216.5 minutes. Lastly, to reach the target point at 22℃, about 154.8 minutes was needed to
complete the process. The trend line of the graph shows declining pattern as the process
undergo filtration and the oil was set to cool. The experiment first started by preheat the
RBD palm oil and then start cooling the oil. There are two processes involve in this
experiment which are crystallization process and filtration process. The crystallization
occurs during the cooling of the palm oil to the desired fractional temperature, holding the
partially crystallized slurry for crystal growth in oil. RBD palm oil was kept homogenized
at about 60℃in homogenizers before the start of crystallization. The heated process was to
decompose any crystal present and to induce crystallization in a proper approach in the
crystallizer. The heated solution was then flowed into the crystallizer (batch type) that was
equipped with mechanical agitator and the temperature inside the crystallizer was
controlled by presence of thermostat. At the end of crystallization process, the solution
consist of a mixture of slurry crystal and liquid oil was formed. The crystallization is very
important because the solid crystal then undergoes filtration process to separate it from
liquid mixture. Next process is filtration process was conducted using an automated
membrane filter that was used to filtrate the oil and separate the solid stearin crystals from
the liquid mixture of olein. The solid stearin crystals were retained as filter cake while the
liquid mixture of the olein passes through the filter as filtrate. Olein yield was maximized
by squeezing the stearin cake through inflation of the membrane with air or liquid.

Temperature, agitation and time play crucial role yielding RBDPO olein and
stearin. Crystallization temperature, cooling rate and agitation speed does not affect the
iodine value (IV), solid fat content (SFC), melting point and cooling properties of the
stearin fraction. The stearin fraction was affected by cooling rate that change its slip
melting point (SMP) while olein fraction was affected by crystallization and cooling rate
only and not agitation speed that causes any changes in IV, SMP, SFC, melting and
crystallization behavior (Ab Latip et al., 2013). Temperature play a great role in yielding
RBDPO olein and stearin as the temperature was used to heat the feedstock solution to
ensure there are no crystal presence inside. Temperature also was manipulated to get the
formation of crystal during cooling when temperature hits low temperature. During the
process, agitator was adjusted to help fulfil the requirement of the crystal formation. The
agitation speed also needs to be adjusted, if the agitation is too fast, the swirling effect will
eradicate the formation of the crystal entirely and if the agitation is too slow the formation
of the crystal will decelerate. Right speed of agitation was needed to have homogenous
temperature in the reactor without breaking the crystal that being formed.

Next, each sample for RBD Palm Oil Feed, RBD Palm Olein and RBD Palm
Stearin has to be in triplicate and undergoes iodine value analysis. Iodine value can be used
to measure the degree of unsaturation of oils and fats. The results are normally expressed as
the number of grams of iodine absorbed by 100g of oil or fat, considering the conditions of
the test. This parameter is extremely important in the palm oil industry, where it is used to
follow the fractionation process. The protocol for iodine value determination usually
comprises a titration procedure, such as the Wijs method. In this procedure, iodine chloride
is used for double-bond saturation analysis, and the content of consumed iodine is
measured by titration with 0.1mol L-1 sodium thiosulfate solution (Wellington, Daniela &
Cristiano, 2019). The results were calculated and recorded for each sample. Based on Table
2, 3 and 4, the results show the volume of thiosulphate solution used for blank solution
(V1) and determination (V2), mass of sample test and iodine value. The average iodine
value calculated for Palm Oil Feed, Palm Olein and Palm Stearin were 51.18, 57.95 and
46.74 respectively. All samples provide iodine values which indicate the presence of
unsaturated oil. Unsaturated oil has more than two bonds which are very reactive towards
iodine (Gregerson, 2019). Palm Olein has the highest iodine value while Palm Stearin has
the lowest iodine value compared to the three samples. Theoretically, iodine value for
Palm Olein should be higher than the Palm Oil Feed because it has higher degree of
unsaturation and fully liquid form at ambient temperature. Based on theory for Palm Stearin,
the mean iodine value has to be lower than Palm Oil Feed. This is because the stearin is a
solid fraction from the fractionation of palm oil (MPOB, n.d.). This show that the result for
iodine value for each sample follow the theory given.

The result of iodine value was compared to the standard value of refinery quality
from Appendix 1. The iodine value for Palm Olein and Palm Stearin was 57.95 and 46.74
respectively. Based on Appendix 1, the given iodine value for Palm Olein is 57 % in 9
hours process cycle which similar to results obtained. For Palm Stearin, the given iodine
value is 34% which lower than result obtained. This is due to presence of unsaturated oil
left in stearin make the degree of unsaturation become higher thus that affecting the iodine
value. Next, production yield % can be calculated using formula = [(weight of olein
produced/weight of RBDPO feed) x 100%]. The efficiency of the plant is measured by the
production yield. From result, the weight of olein is 4 kg while weight of RBD Palm Oil
Feed id 8 kg. The production yield obtained from this plant is 50%. The yields for
fractionation plant producing RBD palm olein from RBD palm oil normally between 78- 80
(%). Production yield obtained was lower than theory at difference of 28-30 (%). This
might be because of many times continuous process running which can reduce the accuracy
and efficiency of the result.
 There are many possible error and recommendations in order to improve the results
of the experiment. Firstly, the oil sample is still in liquid form. As recommendation, make
sure to melt and filter the oil sample to remove any solid impurities and last trace of
moisture. Next, the temperature does not reach 68℃ to 71℃ after the filtration. Thus, the
temperature needs to achieve and maintain at the reference temperature in order to get
accurate iodine value of sample.
CONCLUSION AND RECOMMENDATION
The main objective of the experiment is to perform separation of palm olein and
palm stearin from RBD palm oil via dry fractionation. In the experiment, the analysis was
done to obtain the iodine value of the processed RBD oil. Based from the result, it can be
concluded that the RBD palm oil feed, RBD palm oil olein and RBD palm oil stearin does
not follow the theoretical range value. This might be because of many times continuous
process running which can reduce the accuracy and efficiency of the res

There is some experimental error that may affect the result of the experiment.
Therefore, make sure to perfectly melt and filter the oil to remove any solid impurities and
last trace of moisture. Next, the temperature needs to achieved and needed to maintain at
the reference temperature in order to get accurate iodine value sample. Student should
always keep the temperature of the machine under surveillance as it will also affect the
result of the experiment.
REFERENCES

1. Eric Gregerson (Ed.). (2019). Iodine value. Retrieved from

https://www.britannica.com/science/iodine-value.
2. Hosch, W. L. (n.d.). Nucleation. Retrieved from
https://www.britannica.com/science/nucleation.
3. Latip, R. A., Lee, Y.-Y., Tang, T.-K., Phuah, E.-T., Lee, C.-M., Tan, C.-P., & Lai,
O.-M. (2013). Palm-based diacylglycerol fat dry fractionation: effect of
crystallisation temperature, cooling rate and agitation speed on physical and
chemical properties of fractions. PeerJ, 1. doi: 10.7717/peerj.72
4. MPOB. (n.d.). About Palm Oil. Retrieved from
http://www.palmoilworld.org/about_palmoil.html
5. Timms, R. E. (2005). Fractional crystallisation - the fat modification process for the
21st century. European Journal of Lipid Science And Technology, 107(1), 48–57.
doi: 10.1002/ejlt.200401075
6. Wellington da Silva Oliveira, Daniela Andrade Neves & Cristiano Augusto Ballus.
(2019). Mature chemical analysis methods for food chemical properties evaluation.
Retrieved from https://doi.org/10.1016/B978-0-12-814217-2.00005-6
Appendix

Production Yield:

𝑊𝐸𝐼𝐺𝐻𝑇 𝑂𝐹 𝑂𝐿𝐸𝐼𝑁 𝑃𝑅𝑂𝐷𝑈𝐶𝐸𝐷

𝑷𝒓𝒐𝒅𝒖𝒄𝒕𝒊𝒐𝒏 𝒀𝒊𝒆𝒍𝒅 = × 100°𝐶
𝑊𝐸𝐼𝐺𝐻𝑇 𝑂𝐹 𝑅𝐵𝐷𝑃𝑂 𝐹𝐸𝐸𝐷
4.0 𝑘𝑔
𝑷𝒓𝒐𝒅𝒖𝒄𝒕𝒊𝒐𝒏 𝒀𝒊𝒆𝒍𝒅 = × 100°𝐶
8 𝑘𝑔
𝑷𝒓𝒐𝒅𝒖𝒄𝒕𝒊𝒐𝒏 𝒀𝒊𝒆𝒍𝒅 = 50.0 %

Iodine Value:
12.69 𝐶 (𝑣1 − 𝑣2 )
𝑰𝒐𝒅𝒊𝒏𝒆 𝑽𝒂𝒍𝒖𝒆, 𝑰𝑽 =
𝑀

C: concentration of the sodium thiosulphate solution (mol/L)

V1: volume of sodium thiosulphate used for blank sample (ml)
V2: volume of sodium thiosulphate used for determination (ml)
M: mass of the test sample
For RBD Palm Oil Feed

Sample Calculation

1 12.69 (0.1) (43.3 − 34.5)

𝐼𝑜𝑑𝑖𝑛𝑒 𝑉𝑎𝑙𝑢𝑒, 𝐼𝑉 =
0.2
= 55.84

2 12.69 (0.1) (43.3 − 36.4)

𝐼𝑜𝑑𝑖𝑛𝑒 𝑉𝑎𝑙𝑢𝑒, 𝐼𝑉 =
0.2
= 43.78

3 12.69 (0.1) (43.3 − 34.8)

𝐼𝑜𝑑𝑖𝑛𝑒 𝑉𝑎𝑙𝑢𝑒, 𝐼𝑉 =
0.2
= 53.93
 For RBD Palm Olein

Sample Calculation

1 12.69 (0.1) (43.3 − 34.2)

𝐼𝑜𝑑𝑖𝑛𝑒 𝑉𝑎𝑙𝑢𝑒, 𝐼𝑉 =
0.2
= 57.74

2 12.69 (0.1) (43.3 − 33.6)

𝐼𝑜𝑑𝑖𝑛𝑒 𝑉𝑎𝑙𝑢𝑒, 𝐼𝑉 =
0.2
= 61.55

3 12.69 (0.1) (43.3 − 34.7)

𝐼𝑜𝑑𝑖𝑛𝑒 𝑉𝑎𝑙𝑢𝑒, 𝐼𝑉 =
0.2
= 54.57

For RBD Palm Stearin

Sample Calculation

1 12.69 (0.1) (43.3 − 36.8)

𝐼𝑜𝑑𝑖𝑛𝑒 𝑉𝑎𝑙𝑢𝑒, 𝐼𝑉 =
0.2
= 41.24

2 12.69 (0.1) (43.3 − 35.2)

𝐼𝑜𝑑𝑖𝑛𝑒 𝑉𝑎𝑙𝑢𝑒, 𝐼𝑉 =
0.2
= 51.39

3 12.69 (0.1) (43.3 − 35.8)

𝐼𝑜𝑑𝑖𝑛𝑒 𝑉𝑎𝑙𝑢𝑒, 𝐼𝑉 =
0.2
= 47.59