EXPERIMENT No: 1

PHYSICAL REFINING OF CRUDE PALM OIL

1.0 INTRODUCTION
All crude fats and oils obtained after rendering, crushing or solvent extraction inevitably
contain variable amount of non tryglycerides, components such as fatty acids, mono and
diglycerides, phospatides, sterols, tocopherols, hydrocarbons, pigment(gossypol,chlorophyll),
vitamins(carotene), sterol glucosides and glycolipids.
Physical refining was utilized as early as 1930 as a process for the preneutrallization of
products with a high initial FFA content. In this case, preneutralization was followed by caustic
refining. Later, it was found possible to physically refine lauric oils and tallow if the proper
pretreatment was applied before steam distillation. Physical refining became a reality in the
1950s for processing palm oil, which typically contains high FFAs and low gum contents. The
palm oil process subjected the crude feedstock first to pretreatment and then to deacidification.
The pretreatment consisted of a degumming step and an earth bleaching step, which together
remove certain nonvolatile impurities by filtration. Volatile and thermally labile components
are removed during the conditions of steam distillation under vacuum, which originally gave
the process its name of steam refining. However, for vegetable oils, such as soybeans, that
contain relatively low levels of FFA.
The traditional edible oil processing system consists of caustic neutralization,
bleaching, and deodorization. Caustic neutralization of vegetable oils with high phosphatide
contents delivers a soapstock that is a mixture of sodium salts of fatty acids, neutral oil, water,
unused caustic, and other compounds resulting from the reactions of the caustic with various
impurities in the oil. Disposal of this soapstock or the waste streams from soapstock processing
systems has become increasingly more expensive. A second problem associated with chemical
neutralization is the loss of neutral oil, which reduces the overall yield from the crude oil.
Elimination of the caustic refining step is economically attractive, but it means that degumming
or some other pretreatment process or system must assume all the functions of the alkali
refining process, except for FFA removal.

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 EXPERIMENT No: 1
PHYSICAL REFINING OF CRUDE PALM OIL

2.0 METHODOLOGY

The experiment can be divided into 3 main parts:

1. Removal of free fatty acids, phospholipids and impurities.
2. Removal of pigments, oxidation products, metals and soup.
3. Removal of free fatty acids and fatty acids, mono & diglycerides, oxidation
products, pigments and decomposition products.

The main objective of this experiment is to operate pilot scale experiment of refine,
bleach and deodorize processing of crude palm oil. The experiment starts with identification of
optimal parameter for degumming, bleaching and deodorization processes. The optimal
parameter is identified in range as below:
.
Parameters Degumming and Deodorization(Range)
Bleaching(Range)
Temperature (oC) 80-110 220-260
Pressure (mmHg) 60-90 5-20

Contact time (minutes) 20-50 30-60

After the operating parameters have been identified, a pilot scale experiments facilities
will be set up based on the operating parameter. There are two physical pilot will be used which
are pre-treatment consists of degumming and bleaching stage and deodorization stage. The
neutralization/the pre-treatment stage is done by using the portable container unit. Then
analysis is done for the oil before and after the experiment.

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 EXPERIMENT No: 1
PHYSICAL REFINING OF CRUDE PALM OIL

2.1 Operating Parameter

In this experiment, students need to identify the optimal operating parameters of
refining process. Based on the range of operating parameters given in the previous table
process, students need to select different value of each trial.

Table 2.1: Operating parameter data sheet

Parameters Degumming Bleaching Deodorization
Temperature (oC)
Pressure (mmHg)
Contact time (min)

2.2 Crude Palm Oil Sample

The crude palm oil (CPO) samples used in this research study were obtained from
Kilang Sawit Hutan Melintang Perak. The quality of the CPO sample is good which is the free
fatty acid content of this sample is less than 2.5 % and the moisture content of the sample is
about 0.15 %.

2.3 Phosphoric Acid and Bleaching Earth

Bleaching earth used is neutral bleaching earth and phosphoric acid used is phosphoric
acid 85% concentrated. The dosage of bleaching earth is 1.0% - 3.0% by weight of oil and the
phosphoric acid dosage is 0.5%- 2.0% by weight of oil depends on the FFA % at initial stage.

2.4 Degumming and Bleaching Experiment

The degumming and bleaching experiment are set up according to the optimal
parameter identified, which are ___oC, under vacuum of ___mmHg and contact time of ____
minutes. The equipment set up for this experiment is as shown in Figure 2.1 next page.

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 EXPERIMENT No: 1
PHYSICAL REFINING OF CRUDE PALM OIL

Control panel

Stirrer
rotor

Vaccum valve

Bleaching Filter

Vacuum gauge

Figure 2.1 Bleaching Unit

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 EXPERIMENT No: 1
PHYSICAL REFINING OF CRUDE PALM OIL

2.4.1 Experimental Procedure for Degumming and Bleaching

In this study, the CPO sample used for degumming and bleaching processes is 10000
gram 10 gram for each trial. The phosphoric acid used is about 0.1 % w/w and the
bleaching earth used is about 1 % w/w. Heating element for this experiment is silicon oil.
The CPO is initially heated up to 65-90 oC using water bath. After heating up for 30
minutes, CPO will be transferred to main vessel body T 141 at Bleaching Pilot Plant Unit. The
procedure must be doing through the hose given with initial vacuum condition in T141. Start
stirrer and set the rotation speed accordingly with low rpm. Once the CPO has fully charged
into the vessel, prepare the Phosphoric Acid (PA) with the calculated volume based on the
theory given in the previous page. Transfer PA into T141 slowly through with the same inlet
of CPO previously. Set the time of 30 minutes with constant speed of stirrer. The process can
be done in atmospheric pressure.
Once the degumming process completed, set the vacuum to ____ mmHg. At the same
time, the mixture is heated up to 90oC by manipulating ball valve S141 BV 1555. Once the
vacuum reading is consistent, prepare the bleaching agent based on the weight % provided.
After achieve 30 minutes of degumming, slowly add bleaching powder through suction hose
attached at small tank T 142 similar to CPO and PA charge in process. Let the temperature
reach at desire state and reserve it for one hour or extra another 30 minutes.
Stop the stirrer after that and check the filtration unit to ensure the tightness of thee
filter frame. Run the filtration pump and same time bleed for 10 seconds to reduce vacuum
condition. Open the bottom valve to allow the flow of mixture. The process may be sluggish
due to small diameter of pipe and also the size of the filter cloth which is between 0.5-3.5
micronmeters. Collect the bleach oil in plastic pale and ready to transfer to deodorization pilot
plant unit.

2.5 Deodorization Experiment

The deodorization experiment is set up according to the optimal parameter identified,
which are ____ oC, under vacuum of ___ mmHg and contact time of _____ minutes. The
equipment set up for this experiment is as shown in Figure 2.2 next page.

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 EXPERIMENT No: 1
PHYSICAL REFINING OF CRUDE PALM OIL

Figure 2.2 Deodorization Unit

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 EXPERIMENT No: 1
PHYSICAL REFINING OF CRUDE PALM OIL

2.5.1 Experimental Procedure for Deodorization

After the oil has undergone degummed and bleached process, the oil is then will be
prepared to deodorization process.
Place a new filter bag in polishing filter F08I and close the filter. Start vacuum system
V08I following the procedure outlined in the instruction manual and evacuate deodorizer D08I
to a vacuum of about 6.7 mbar.
Start pump P704 (located at the storage tank area) and feed oil from the storage tank to
deodorizer D08I. At high level HLA08I, stops pump P704. Switch on electrical heating
element HT08I. Set the deodorization temperature (normally 250C) at temperature controller
TIC08I.
Use the metering valve to set the flowrate of sparging steam to deodorizer D08I (see
Appendix 1). Maintain the oil in deodorizer D08I at the deodorization temperature and under
steam sparging for the desired deodorization time. At the end of the deodorization time, switch
off electrical heating element HT08I and stop temperature controller TIC08I.
Start cooling water flow to the internal cooling coil of deodorizer D08I to cool down
the oil to less than 90C. Stop cooling water flow and the temperature controller, close the
sparging steam valve and shut down vacuum system V08I. Open the vent valve of deodorizer
D08I to break the vacuum. Starts pump P08I and discharge the oil to storage tank T082 through
polishing filter F08. When deodorizer D08I is empty, stop pump P08I. Empty the pipelines by
opening the drain valve at the pump.

3.0 Analysis
The experiments for CPO and RBDPO qualities are conducted based on the standard
method by MPOB. The following analysis should be done to determine the quality of oil
(before and after the process):
a) Free Fatty Acid (FFA) content
b) Moisture content
Sampling standard must be followed and data must be taken at least 3 trials. Data
analysis should be conducted to find mean and median. For crude palm oil, sample should be
taken from bottom, middle and top drum. The sample are mixed and taken for analysis.

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 EXPERIMENT No: 1
PHYSICAL REFINING OF CRUDE PALM OIL
For process oil, sample should be taken uniformity at sampling valve. Sample should
be taken for the first time after processing.

3.1 Free Fatty Acids (FFA) Content

Theory:
Acidity or free fatty acid (FFA) in the palm oil is calculated as palmitic acid from the
equation:

25.6
% Free Fatty Acid as palmitic acid =

Where,
M is the molarity of standard NaOH or KOH solution
V is the volume of the standard NaOH or KOH solution used (ml)
m is the mass of the test sample (g)

Apparatus:
Burette, 25 ml capacity graduated in 0.05 ml subdivisions
Conical flasks, 250 ml and 500 ml
Hot plate, with magnetic stirrer and temperature control
Analytical balance

Reagents:
1. Standard potassium or sodium hydroxide, 0.1M
Potassium or sodium hydroxide of approximate 0.1M should be standardized
with potassium hydrogen phthalate.

Dry potassium hydrogen phthalate in an oven at 120oC for 2 hr and allow

cooling in a desiccators before use.
Weight 0.4g 0.02g to 0.1 mg accuracy of the potassium hydrogen
phthalate directly into a conical flask.
Add 50 ml of water and a few drop of phenolphthalein indicator.
Place on a hot plate and swirl till the salt has completely dissolved and
titrate with potassium or sodium hydroxide to the first appearance of a
permanent pink color.
103
Molarity of the alkali = 204.2

2. Phenolphathlein indicator solution, 1% in isopropanol (or in 95% ethanol)

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 EXPERIMENT No: 1
PHYSICAL REFINING OF CRUDE PALM OIL
3. Neutralized isopropanol

Place 50 ml isopropanol in a flask and bring the solution to the boil over
hot plate.
Add about 0.5 ml of phenolphthalein and neutralized by drop-wise
addition of 0.1M potassium hydroxide or sodium hydroxide till a faint
but permanent pink color is obtained.

Experimental procedures:
1. Prepare the sample for the analysis by melting the sample at 60 to 70 oC and
thoroughly homogenize it before sampling.
2. Keep the sample in a clean and dry flask with stopper or screw cap to prevent
contact with humidity.
3. Weigh 5 to 6 g of sample into a conical flask.
4. Add 50 ml of the neutralized solvent.
5. Place the flask on the hot plate and regulate the temperature to about 40oC.
6. Shake the sample gently while titrating with standard alkali until the appearance
of the first permanent pink color. The color must persist for 30 sec.

3.2 Moisture Content

Theory:
The moisture content can be calculated by the equation below:

% Moisture and volatile matter = 100%

Where,
m is the mass of the dish (g)
mb is the mass of the dish and test sample (g)
md is the mass of the dish and test sample after drying (g)
Apparatus:
Air oven
Analytical balance
Petri dishes

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 EXPERIMENT No: 1
PHYSICAL REFINING OF CRUDE PALM OIL

Desiccator

Experimental procedures:
1. Dry cleaned petri dishes in the oven at 103oC for at least 15 min and allow
cooling in desiccators. Weigh the dish to the nearest 0.001g.
2. Weigh approximately 10g of the molten oil (test sample) to the nearest 0.001g
into the dish. Return to the desiccators until the oil has thoroughly cooled.
Weigh the dish plus the oil to the nearest 0.001g and place the dish in the
middle shelf of the oven at 103oC for exactly 2.5h.
3. Remove the dish and allow it to cool to room temperature in the desiccators
(30 to 45 min) before reweighing to the nearest 0.001g.
4. If the moisture exceeds 0.3%, continued drying (at 30 min interval) to constant
weight is recommended. In this case, the difference between two successive
weighing should not exceed 0.002g. Carry out two determinations of test
portions taken from the same test sample.

Table of Data:
Free Fatty Acids analysis
Table 1: Result for FFA analysis (CPO)
Crude Palm Oil Volume of Mass of test FFA value (%)
(CPO)
standard NaOH sample, m (g)
or KOH used, V
(ml)
Sample 1

Sample 2

Sample 3

Average

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 EXPERIMENT No: 1
PHYSICAL REFINING OF CRUDE PALM OIL

Table 2: Result for FFA analysis (RBDPO)

Refined Bleached Volume of Mass of test FFA value (%)
Deodorized Palm standard NaOH sample, m (g)
Oil (RBDPO) or KOH used, V
(ml)
Sample 1

Sample 2

Sample 3

Average

Moisture Content Analysis

Table 3: Result for moisture analysis (CPO)
Crude Palm Mass of dish, Mass of dish + Mass of dish + Moisture content (%)
Oil (CPO) m (g) sample before sample after
drying, mb (g) drying, md (g)
Sample 1

Sample 2

Sample 3

Average

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 EXPERIMENT No: 1
PHYSICAL REFINING OF CRUDE PALM OIL
Table 4: Result of moisture analysis (RBDPO)

Refined Bleached Mass of dish, Mass of dish + Mass of dish + Moisture content
Deodorized Palm m (g) sample before sample after (%)
Oil (RBDPO) drying, mb (g) drying, md (g)
Sample 1

Sample 2

Sample 3

Average

#Show sample of calculation for each analysis. Find the standard deviation of each data and
present in the table.

4.0 Discussion
1. Explain the principle of degumming, bleaching and deodorization in this experiment.
2. Compare and explain the result of FFA analysis and moisture content analysis of RBDPO
with the standard value of refinery quality (refer Appendix 1). Justify your explanation.
3. Compare and explain the result of FFA analysis and moisture content analysis of CPO with
the RBDPO. Justify your explanation.
4. Discuss any possible errors in the experiment and state any recommendation to improve the
result.

#Show the calculation on how to prepare phosphoric acid and bleaching earth in the appendix
of your lab report.

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 EXPERIMENT No: 1
PHYSICAL REFINING OF CRUDE PALM OIL
APPENDIX 1
Table A1: Desired quality of pretreated and RBD Palm Oil

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