CHEMISTRY OF FATS AND OILS

(SCH 4432)

LABORATORY REPORT

EXPERIMENT 1: DETERMINATION OF IODINE VALUE BY

USING WIJS-CYCLOHEXANE METHOD

NAMES MATRIC NO
1 NUR SHAFINA BINTI MOHD NOR 1616910
2 MUHAMMAD IBRAHIM FIKRI BIN RAWI 1617549

PROGRAMME : BACHELOR OF SCIENCE (APPLIED CHEMISTRY)

INSTRUCTOR’S NAME : ASST. PROF. DR. MOHAMAD WAFIUDDIN BIN ISMAIL

DATE OF EXPERIMENT : 13TH FEBRUARY 2018 (WEDNESDAY)

DATE OF SUBMISSION : 20TH FEBRUARY 2018 (WEDNESDAY)

SEMESTER : 2 (2018/19)

OBJECTIVES
  To determine the iodine values of sunflower oil, palm oil and coconut oil by using
cyclohexane method.

 To estimate the unsaturation level of sunflower oil, palm oil and coconut oil.

 To study about Wijs-cyclohexane method.

INTRODUCTION

Fats and oils are made up of three elements: carbon, oxygen and hydrogen, where these
elements were combined to form fatty acids chain. Three of these chains joined together to
form triglyceride molecule of which this molecule is the basis of all oils and fats.

Figure 1: Structure of triglyceride.

Fatty acids can be classified into saturated or unsaturated: saturated fatty acids contain
only single bond between the carbon atoms while unsaturated fatty acids contain one or more
double bonds in between the carbon atoms in addition to the single bonds present in the fatty
acid chain.

Unsaturated fatty acids can be harmful in the double bonds present are in the trans-
form although the naturally occurring unsaturated fats are in the cis- form. Trans fatty acids
are associated with risky health problems particularly cardiovascular diseases.

One of the several different methods to check the unsaturation level in fatty acids is
by determining the iodine value of fats and oils. Iodine value (IV) is a measure of the degree
of unsaturation in fats and oils components, as determined by the uptake of halogen. A higher
IV indicates a higher degree of unsaturation in the fats and a higher susceptibility to
oxidation. It can also be defined as the number of grams of iodine consumed by 100g of fats,
apart from an indication of fat’s susceptibility to be oxidized as it measures the reaction of

2
iodine with the double bonds of unsaturated fatty acids. As fats with more double bonds
provide more sites for oxidation, the iodine value of a fat helps predict fat stability.

In this experiment, we will measure the IV of three different oil samples: sunflower
oil, palm oil and coconut oil by using Wijs-cyclohexane method. Generally, through this
method, excess of Wijs solution is added to a solution of oil dissolved in cyclohexane. Wijs
solution is a stable solution consisting of iodine monochloride (ICl) in acetic acid that
halogenates the double bonds in the fat. Then, the excess halogen is reduced with potassium
iodide and finally titrated with standard sodium thiosulphate using a starch indicator.

MATERIAL AND APPARATUS

3
 MATERIALS APPARATUS
Oil samples: sunflower oil, palm oil, coconut oil Pipette
Wijs solution Erlenmeyer flask with glass stopper
Potassium iodide solution Measuring cylinders
Cyclohexane solution Dropper
Starch indicator solution Weighing balance
Sodium thiosulphate solution
Distilled water

Figure 2: Erlenmeyer flask with glass stopper

EXPERIMENTAL PROCEDURE

1. 0.5g of each oil sample were accurately weighed in an Erlenmeyer flask.

2. 20mL of cyclohexane was added to the flask. The flask was slightly warmed on a
heating pad for a short period.

4
 3. 25mL of Wijs solution was added to the flask and stoppered. The flask was gently
shaken and placed in a dark cupboard for 1 hour.

4. 20mL of KI solution and 100mL of water were added consecutively.

5. The solution was titrated with Na2S2O3 solution while the flask was carefully shaken
until the yellow colour almost disappeared.

6. 5 drops of starch indicator solution were added into the solution and the titration was
continued until the blue colour disappeared.

7. For each step, any observations were recorded. For each sample, the iodine value
determination test was repeated twice.

8. A blank test was carried out simultaneously under the same conditions.

DATA AND RESULTS ANALYSIS

DISCUSSION

5
CONCLUSION

In conclusion, the higher the iodine value, the higher the degree of unsaturation of fatty acids.

////////////////////////////////////OOOOO//////////O/OOOOOOO

QUESTIONS

1. What is the relationship between iodine value (IV) and the stability of fats and
oils?

6
The higher the IV, the greater the number of double bonds which will lead to a higher degree
of unsaturation of fatty acids, where the higher the chances of oxidation upon exposure to
open air. Hence, the lower the stability of fats and oils.

2. Explain how IV is used to monitor the progress of hydrogenation.

Hydrogenation is a reduction reaction of double or triple bonds in hydrocarbon which results

in an addition of hydrogen. We can monitor the progress of hydrogenation by the iodine
value, where the higher the IV, the higher the degree of unsaturation hence indicates the
higher number of double bonds. A higher number of double bonds signals a slow progress of
hydrogenation and vice versa.

3. Besides IV, name other methods used in industry to monitor hydrogenation

process.

- A combination of size exclusion chromatography (HPLC-SEC) with refractive index (RI)

and diode array detection (DAD).[5]

- A development of NMR method that is based on the determination of a monoexponential

approximation of the longitudinal relaxation time, T1, which is shown to be highly correlated
with the iodine number.[6]

REFERENCES

1. Sue, T T. Determination of Iodine Values of Palm Oil and Palm Kernel Oil Products
Using Non-Chlorinated Solvents. PORIM Bulletin, 31. Retrieved from
http://palmoilis.mpob.gov.my/publications/OPB/opb31-tang.pdf

7
2. Iodine Value. Retrieved from https://mantech-inc.com/wp-
content/uploads/2016/08/AN-Iodine-Value.pdf
3. T.H. Sanders. (2003). Encyclopaedia of Food Sciences and Nutrition, 2.

4. Chemistry of Oils and Fats. National Edible Oil Distributors Association.

5. Varotsis, N. (1997). An Analytical Method for Rapid Monitoring of the Degree of

Hydrogenation of Recycled Lubricating Motor Oils. American Chemical Society, 36
(9), pp 3915–3919.
6. Khaloui, M. (1990). Monitoring hydrogenation in the margarine industry by low
resolution pulsed NMR. Journal of the Science of Food and Agriculture, 53(3), pp
389-393.