JAN 2016

EXPERIMENT No: 3
LAB SCALE MARGARINE PRODUCTION

1.0 OBJECTIVES

The objectives of this experiment are:

 To produce margarine using basic formulations from palm oil.
 To study relationship between physical and chemical properties of margarine with
raw material.

2.0 INTRODUCTION

Margarine was first manufactured in 1869 by a French chemist; Hippolyte Mege Mouries.
The fundamental of margarine is a combination between two phases; 80% of oil phase (fat
blend) and 16% of aqueous phase. Margarine which contains 80% of fat blend has
microstructure of water-in-oil (W/O) emulsion that contributes dispersed water droplets of
typically 5 to 10 μm diameters. This emulsion was formed with the help of emulsifier such as
lecithin and monoglycerides. Today’s margarine can be formulated from any variety of
animal or vegetable fats. Margarine is often mixed with skimmed milk, salt and emulsifiers.
Furthermore, margarine that is made from vegetable oils is highly in demand in today’s
market value due to health purpose.

3.0 METHODOLOGY
3.1 Material and Apparatus
The material and apparatus required for this experiment are listed below:
Material Apparatus
RBD Palm Oil (A) Homogenizer (Model Silverson SL2T)
RBD Palm Stearin (B) 2000 ml beaker for ingredients mixing
Salt 5000 ml beaker for water bath
Water Hot plate
Emulsifier Magnetic stirrer

.
3.2 Formulation
The formulation of margarine production as below:

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EXPERIMENT No: 3
LAB SCALE MARGARINE PRODUCTION

Table 1: Formulation Margarine A

Material Percentage (%)

RBD Palm Oil (A) 65.00

RBD Palm Stearin(B) 15.00

Emulsifier 0.20

Water 16.00

Salt 3.80

Color (Beta carotene) -

TOTAL 100.00

Table 2: Formulation Margarine B

Material Percentage (%)

RBD Palm Oil (A) 60.00

RBD Palm Stearin (B) 11.00

Emulsifier 0.20

Water 25.00

Salt 3.80

Color (Beta Carotene) -

TOTAL 100.00

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3.3 Experimental Procedure

3.3.1. Setup the instrument as shown in Figure 1.

1. Homogenizer (Model Silverson SL2T)

2. Switch on/off button

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LAB SCALE MARGARINE PRODUCTION

3. Stirrer speed controller

4. Stirrer speed monitor
5. Height adjust knob
6. Stirrer
7. Clipper
8. 2000 ml beaker for ingredients mixing
9. 5000 ml beaker for water bath
10. Hot plate magnetic stirrer
11. Heat controller

3.3.2 As the instrument was setup, mix together the oil to form fat blend. Heat the fat
blendbetween 50oC – 55oC.

3.3.3 After the oil was uniformly mixed, take a bit of blend sample for Slip Melting Point
(SMP) analysis.

3.3.4 Later, add emulsifier into the fat blend with color and flavor. Set the speed of
homogenizer between 300 rpm to 700 rpm. Stir the fat blend until all emulsifier
diluted.

3.3.5 Next, add the aqueous phase ingredients that had been mixed before into the fat blend
and continuously stir the mixture until emulsion was formed.

3.3.6 Stir the emulsion until it was uniformly mixed. Then, setup the cooling instrument as
shown in Figure 2.

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EXPERIMENT No: 3
LAB SCALE MARGARINE PRODUCTION

1. Retort stand
2. Thermometer
3. Aluminium bowl with ice
4. 2000 ml beaker
5. Clipper

3.3.7 The beaker used must be clean and empty. Cool the beaker until it was 5 oC to 10oC.
Later, pour the hot emulsion into the cooled beaker and stir continuously until the
semisolid formed.

3.3.8 Pack the semisolid emulsion into plastic packaging and then stored in refrigerator for
one day (24 hours). This step is known as tempering. After one day, take out the
product from the refrigerator and store in room temperature.

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LAB SCALE MARGARINE PRODUCTION

4.0 ANALYSIS

4.1 Slip Melting Point (SMP)

Slip Melting Point (SMP) analysis using the MPOB Test Method for SMP is carried out by
capillary technique.

4.1.1 Setup the instrument as shown in Figure 3.

1. Retort stand
2. Thermometer
3. 600 ml beaker
4. Hot plate
5. Capillary tube (both open ended)

4.1.2 Measure and mark 1 cm of capillary tube from open ended capillary tube.

4.1.3 Then, dip the three open ended capillary tubes with internal diameters of 1.1 mm to
1.3 mm and external diameters of 1.4 mm to 1.7 mm in filtered liquid oil so that a
column of fat rise until 1 cm into each tube.

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LAB SCALE MARGARINE PRODUCTION

4.1.4 Chill the tubes immediately against ice, place in a test tube and keep in refrigerator
for 16 hours or minimum 1 hour for tempering process.

4.1.5 After tempering, tie each tube against a thermometer and dip in cold distilled water.
The temperature of water will rise to 1oC/min until the fat in the column begin to rise
past the marking point. The temperature at this point is taken as the SMP.

4.2 Iodine Value

Theory:
The iodine value, IV expressed in grams per 100g of fats by the equation:
12.69C (V 1−V 2 )
Iodine Value, IV =
M

Where,
C is the concentration of the sodium thiosulphate solution (mol/L)
V1 is the volume of sodium thiosulphate solution used for blank sample (ml)
V2 is the volume of sodium thiosulphate solution used for the determination (ml)
M is the mass of the test sample (g)

Apparatus:
 Glass weighing scoops
 Conical flasks, 500 ml capacity fitted with ground glass stoppers and
completely dry.
 Analytical balance

Reagents:
1. Potassium iodide (KI), 100 g/L not containing iodate.
2. Starch solution
 Mix 5g of soluble starch in 30 ml of water and add to 1000 ml of
boiling water.
 Boil for 3 min and allow to cool.
3. Sodium thiosulphate (Na2S2O3.5H2O), standard volumetric solution, c = 0.1M
4. Solvent, prepared by mixing equal volumes of cyclohexane and glacial acetic
acid.
5. Wijs reagent, containing iodine monochloride in acetic acid.

Experimental procedures:
1. Melt the sample, if not already liquid and filter through two pieces of filter paper
to remove any solid impurities and the last trace of moisture.

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LAB SCALE MARGARINE PRODUCTION

2. After filtration, allow the sample to achieve a temperature of 68 oC – 71oC

before weighing the sample.
3. Once the sample has achieved the temperature, immediately
weight the sample into a 500 mL flask.
4. According to the iodine value expected for the sample, weigh to the nearest
0.001g in a weighing scoop. The mass of test sample indicated in Table 1.

Table 1: Mass of test sample

Expected iodine value Mass of test sample Volume of solvent
(g/100g) (g) (ml)
< 1.5 15.00 25
1.5 – 2.5 10.00 25
2.5 – 5 3.00 20
5 – 20 1.00 20
20 – 50 0.40 20
50 – 100 0.20 20
100 – 150 0.13 20
150 - 200 0.10 20

5. Add the volume of solvent indicated in Table 1 on top of the sample and swirl to
ensure the sample is completely dissolved.
6. Add 25 mL of Wijs reagents using the pipette into the flask containing the
sample stopper the flask and swirl to ensure an intimate mixture.
7. Prepare a blank with solvent and reagent but omitting the test sample.
8. Immediately store the flasks in the dark room for the 1 hour at a
temperature of 25oC.
9. Remove the flask from the storage and add 20 mL of potassium iodide (KI),
followed and 150 ml of distilled water.
10. Titrate with standard sodium thiosulphate solution, adding it gradually and with
constant and vigorous shaking. Continue the titration until the yellow color due to
iodine has almost disappeared.
11. Add a few drops of starch indicator solution and continue the titration until the
blue color just disappears after very vigorous shaking.
12. Prepare and conduct at least one blank determination with each group of samples
simultaneously and similar in all aspect to the sample.
13. Take and analyze the sample of each 30 min running hours of fractionation plant.

5.0 Discussion
1. Explain the principle of process involved in margarine production.
2. Compare and explain the result of the slip melting point analysis of raw material with
the
product of margarine. Justify your answer.
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LAB SCALE MARGARINE PRODUCTION

3. Compare and explain the result of the iodine value analysis of raw material with the
product of margarine. Justify your answer.
4. Discuss the quality of margarine from Formulation A and Formulation B and make
comparison.
5. Discuss any possible errors and state any recommendation to improve the process.

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EXPERIMENT No: 3
LAB SCALE MARGARINE PRODUCTION

Table of Data:

Slip melting point analysis

Table 1: Result of SMP analysis for Formulation A

Formulation A Slip Melting Point, T (oC)

Tube 1 Tube 2

Raw material 1:

Raw material 2:

Margarine blend (product)

Table 2: Result of SMP analysis for Formulation B

Formulation B Slip Melting Point, T (oC)

Tube 1 Tube 2

Raw material 1:

Raw material 2:

Margarine blend (product)

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EXPERIMENT No: 3
LAB SCALE MARGARINE PRODUCTION

Iodine value analysis

Formulation A

Table 3: Result of iodine value for Formulation A (Raw Material)

Formulation Volume of sodium Volume of sodium Mass of test Iodine value
A thiosulphate thiosulphate sample, M (g)
(Raw solution used for solution used for the
Material) blank sample, V1 determination, V2
(ml) (ml)
Sample 1

Sample 2

Sample 3

Table 4: Result of iodine value for Formulation A (Product)

Formulation Volume of sodium Volume of sodium Mass of test Iodine value

A thiosulphate thiosulphate sample, M (g)
(Product) solution used for solution used for the
blank sample, V1 determination, V2
(ml) (ml)
Sample 1

Sample 2

Sample 3

Formulation B
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EXPERIMENT No: 3
LAB SCALE MARGARINE PRODUCTION

Table 5: Result of iodine value for Formulation B (Raw Material)

Formulation Volume of sodium Volume of sodium Mass of test Iodine value
B thiosulphate thiosulphate sample, M (g)
(Raw solution used for solution used for the
Material) blank sample, V1 determination, V2
(ml) (ml)
Sample 1

Sample 2

Sample 3

Table 6: Result of iodine value for Formulation B (Product)

Formulation Volume of sodium Volume of sodium Mass of test Iodine value

B thiosulphate thiosulphate sample, M (g)
(Product) solution used for solution used for the
blank sample, V1 determination, V2
(ml) (ml)
Sample 1

Sample 2

Sample 3

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