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LABORATORY REPORT

FST 261 (INTRODUCTION TO FOOD CHEMISTRY)

MEMBERS NAME:
1.
2.
3.
4.

ARIFF ASYRAN B MD SUPIE (2011842178)


MUHAMMAD QUTHAM B KHAIRUDDIN (2011669324)
NUR SYAHIRA BT ABDUL AZIZ (2011418664)
NURALIS ATIQAH BT AMINULLAH (2011424298)

GROUP: AS116 4A2


EXPERIMENT: EXPERIMENT 2; RANCIDITY MEASUREMENT IN
FATS/OILS
DATE OF EXPERIMENT: 11 MARCH 2013
DATE OF SUBMISSION: 19 MARCH 2013
LECTURERS NAME: MISS ROHASMIZAH BT HASHIM
EXPERIMENT 2: RANCIDITY MEASUREMENT IN FATS/OILS

INTRODUCTION
Most any food can technically become rancid. The term particularly applies to oils. Oils
can be particularly susceptible to rancidity because their chemistry which makes them
susceptible to oxygen damage. When food scientists talk about rancidity, they are often talking
about a specific type of rancidity involving oxygen damage to foods, and this type of rancidity is
called "oxidative rancidity." During the process of oxidative rancidity, oxygen molecules interact
with the structure of the oil and damage its natural structure in a way that can change its odour,
its taste, and its safety for consumption.
Oxidation of fats, generally known as rancidity, is caused by a biochemical reaction
between fats and oxygen. In this process the long-chain fatty acids are degraded and short-chain
compounds are formed. One of the reaction products is butyric acid, which causes the typical
rancid taste.
Rancidification is the decomposition of fats, oils and other lipids by hydrolysis or
oxidation, or both. Hydrolysis will split fatty acid chains away from the glycerol backbone in
glycerides. These free fatty acids can then undergo further auto-oxidation. Oxidation primarily
occurs with unsaturated fats by a free radical-mediated process. These chemical processes can
generate highly reactive molecules in rancid foods and oils, which are responsible for producing
unpleasant and noxious odours and flavours. These chemical processes may also destroy
nutrients in food. Under some conditions, rancidity, and the destruction of vitamins, occurs very
quickly.

A. DETERMINATION OF ACID VALUE OR FREE FATTY ACID

OBJECTIVE:
1. To determine the acid value or free fatty acid in two different sample of fats/oils.

PROCEDURE:

25 Ml of diethyl ether is mixed with 25 Ml of alcohol and 1 Ml of 1 % phenolphthalein solution


in a conical flask.

The solution was neutralized with 0.1 M NaOH.

1-10 gram of the oil (palm oil) was dissolved in the mixed neutral solvent.

Titrate with 0.1 M NaOH until a pink colour persists for 15 seconds is obtained.

The procedure was repeated by replacing the palm oil with olive oil.

RESULTS:
TABLE 2.1: ACID VALUE OR FFA OF FATS/OILS

SAMPLE

OLIVE
OIL
PALM OIL

VOLUME OF TITRATION ( ml)

ACID
VALUE

FFA

TRAIL 1
0.3

TRAIL 2
0.2

TRAIL 3
0.2

AVERAGE
0.23

1.1243

0.56210

0.1

0.05

0.1

O.O833

0.0921

0.04605

CALCULATION
PALM OIL
Acid value

titre (mL) x 5.61


Weight of samples

0.0833 X 5.61
5.0760

0.0921

Acid value

2 x FFA

0.0921

2 X FFA

FFA

0.04605

titre (mL) x 5.61


Weight of samples

0.23 X 5.61
1.1477

1.1243

Acid value

2 x FFA

1.1243

2 X FFA

FFA

0.5621

OLIVE OIL
Acid value

DISCUSSION

Separating fatty acids from the fat molecule is called as free fatty acids. Usually, this
separation process already occurs in the plant. Certain biocatalysts or enzymes and further
stimulated by light, water and heat caused this separation process in plant. The acid value is a
measuring amount of free fatty acids content by lipid hydrolysis. This acid value is determined
by titration method which is directly titrating fat/oil in alcoholic medium and sodium hydroxide
solution.
In this experiment, there are two samples that have been used which are olive oil and
palm oil. Both types of oil undergo the same titration method. The titration method is conducted
by three times as wanted to get an accurate result. An average volume of titration and average
weight of samples are taken. From titration method, the acid value and free fatty acid calculated
as oleic acid and palmitic acid.
From table 2.1, the acid value and free fatty acid content in both types of oils is different.
The acid value for olive oil is higher than acid value for palm oil. For free fatty acid content of
olive oil or oleic acid value is 0.5666 gram. This value has the far distinction when compared
with an actual value which is 0.0282 gram. This is because have an error during titrate the oil for
example the reading of volume is not accurate. Next, the free fatty acid content in palm oil is
called as palmitic acid and have 0.0460 gram of palmitic acid. This value can be accepted as not
too far with an actual value which is 0.0256 gram.
There are a few precaution can be taken during handle this experiment. Firstly, during
neutralize the solution before adding the fats/oils, read the volume of solution right and carefully.
Second, during titration method of fats/oils to extract the free fatty acid, the colour changes must
be properly observed. This is because, the colour changes occur very fast and the reading of
volume must be accurate.

CONCLUSION
In conclusion, the acid value and free fatty acid content in olive oil and palm oil are
different where olive oil has high acid value and free fatty acid content compared to palm oil.
Oleic acid is the monounsaturated fats of olive oil can reduce the risk of coronary heart disease,
while palmitic acid can increase blood cholesterol levels and may contribute to heart disease if
excessive intake.

B. DETERMINATION OF PEROXIDE VALUE

OBJECTIVE:
1. To determine the peroxide value in fats/oils.

PROCEDURE:

1 gram of oil (palm oil) is weighed into dry and clean test tube. (best to do in the dark)

1 gram of potassium iodide powder was added into the sample while it is still a liquid. 20 mL of
solvent mixture (Glacial Acetic Acid : Chloroform, 2 : 1 v/v) were added.

The test tube was placed in the boiling water so that the liquid boiled within 30 seconds. (boil
vigorously for not more than 30 seconds).

The test tube content was poured immediately into a conical flask containing 20 mL of 5 %
potassium iodide solution.

The test tube was rinsed twice with 25 mL distilled water and poured back into the conical flask.

The mixture was titrated with 0.002 M sodium thiosulphate solution using starch solution as an
indicator. The flask was evenly shaken.

The steps were repeated again with olive oil. At the same time, the blank determination was
prepared.

CALCULATION

Peroxide value is usually reported as the mL of 0.002 M sodium thiosulphate per gram of
sample. If this value is multiplied by 2, the figure then equals milliequivalents of peroxide
oxygen per kilogram of sample (mEq/kg), which has greater international recognition.
Fresh oils usually have peroxide values below 10 mEq/kg. A rancid taste often begins to be
noticeable when the peroxide value is between 20 40 mEq/kg.
Peroxide Value =
T
Vs
Vb

=
=
=

V sV b
Weight of sample

x T x 103

Molarity of sodium thiosulphate


Volume in mL titration for sample
Volume in mL titration for blank

OLIVE OIL CALCULATION

Peroxide Value

(PV x 2) mEq/kg

3.970.70
1.007

=
=

6.49

6.49 x 2

12.98 mEq/kg

x 0.002 x 103

PALM OIL CALCULATION

Peroxide Value

(PV x 2) mEq/kg

0.730.70
1.003

0.06

0.06 x 2

0.12 mEq/kg

x 0.002 x 103

RESULTS
TABLE 2.2: PEROXIDE VALUE OF FATS/OILS
Volume of titration (ml)
Sample /
Blank

Trial 1

Trial 2

Trial 3

Peroxide
Value (PV)

(PV x 2)
mEq/kg

Average

Blank

1.00

0.50

0.60

0.70

Olive oil

3.80

4.50

3.60

3.97

6.49

12.98

Palm oil

1.10

0.60

0.50

0.73

0.06

0.12

DISCUSSION
Fats and oils play an important role in the flavour, aroma, texture, and nutritional quality of
foods, pet foods, and feeds. They can be added during manufacturing or may be inherent to the
product or ingredient. The product may be pure oil or it may be part of a complex mixture with
proteins, carbohydrates, minerals, and vitamins.
Rancidity is occurred caused by the action of air (oxidative rancidity) or by
microorganisms (ketonic rancidity) in oil. Oxygen is taken up by the fat with the formation of
peroxides in oxidative rancidity. The degree of peroxide formation and the time taken for the
development of rancidity are different among oils. Peroxide value is a measure of the peroxides
contained in the oil. The peroxides present are determined by titration against thiosulphate in the
presence of potassium iodide (KI). Usually, starch solution is used as indicator.
In this experiment, there are two samples that have been used which are olive oil and
palm oil. The peroxide value of these two samples is obtained. Based on the result obtained, the
peroxide value of olive oil is 12.98 mEq/kg which is higher than palm oil, 0.12 mEq/kg. Both of
the oils are not rancid because rancid taste often begins to be occurred when the peroxide value
is between 20 - 40 mEq/kg. While, fresh oil is usually have peroxide value below 10 mEq/kg, so
palm oil is still a fresh oil based on the its peroxide value. As the peroxide values are not static
and care must be taken in handling and testing samples. It is difficult to provide a specific
guideline relating peroxide value to rancidity. High peroxide values are a definite indication of a

rancid fat, but moderate values may be the result of depletion of peroxides after reaching high
concentrations.
Oils can be especially susceptible to rancidity because their chemistry can make them
exceptionally susceptible to oxygen damage. Specific type of rancidity involving oxygen damage
to foods, and this type of rancidity is called "oxidative rancidity." Oxidative rancidity occurs
when the double bonds of an unsaturated fatty acid react chemically with oxygen. During the
process of oxidative rancidity, oxygen molecules interact with the structure of the oil and damage
its natural structure in a way that can change its odour, its taste, and its safety for consumption.
Chemical reaction produces butyric acid which gives the foul smell and taste.
Last but not least, there are some precautions that can be taken during conducting this
experiment. We should not add fresh oil to vessels that containing old oil. The old oil will trigger
a reaction and the new oil will become rancid far more rapidly than if the oil was stored in a
clean empty vessel. Other than that, avoid using vessels that are wet, this will also speed up the
problems associated with oxidation, we have to allow the tanks to drain and dry adequately
before use.

CONCLUSION
In conclusion, the peroxide value of olive oil is higher than palm oil. Palm oil can be state
as fresh oil as its peroxide value is less than 10. In addition, rancidity has three types which are
hydrolytic rancidity, oxidative rancidity and microbial rancidity.

QUESTION:
1. What is rancidity?
Rancidity is the edible oils, fats and their food products on storage that show
deteriorationwhich is occurred by the development of off-flavour, off-odour and some
timeschange in colour and taste in the fatty food products. This change occurs as soon asthe
oils, fats and fatty food products come into contact with atmospheric oxygen.The enzymes
and micro-organisms also react with them and bring about alteration inthe structure of oils
and fats.
2. List 2 types of rancidity which normally occur in food products.
Hydrolytic rancidity
Oxidative rancidity
3. What are the factors that encourage the rancidity of fats and oils?

The factors that encourage the rancidity of fats and oils are oxidation process and hydrolytic
process and sometimes it can be both.

REFERENCE

Determination of Acid Value. (2012). In: Manual methods of Analysis of Foods.


Retrieved from http://fssai.gov.in/Portals/0/Pdf/15Manuals/OILS%20AND%20FATS.pdf

Rancidity in fats and oil. (n.d.). Retrieved March 15, 2013 from
http://www.shumaonline.com/bakeryarticle-foodsafety-rancidity.html

Methodology for Lipids. (n.d.). Retrieved March 15, 2013 from


http://www.eplantscience.com/index_files/plant%20protocols/Lipids/determination_of_p
eroxide_value.php

Steele R., (2004), Understanding And Measuring The Shelf-Life Of Food,


Woodhead Publishing Limited
David B. M., (1985), Flavour Chemistry of Fats and Oils, American Oil
Chemists Society.
Norman N.P. and Joseph H. H., (1995), Food Science 5 th edition , Aspen
Publishers Inc.
Rancidity In Foods, (2009), retrieved 17 March 2013 from
http://www.cip.ukcentre.com/Rancidity.htm