INSTRUCTION

Oils and fat quality. Lipid oxidation.

Determination of peroxide value in fats and oil.

It is arguable that the two most important chemical reactions that occur in food systems are
lipid oxidation and non-enzymatic browning. This lab exercise focuses attention on the former
reaction. Lipid oxidation, which is also called auto-oxidation, occurs in lipid material by way
of a free-radical mechanism. After an induction period, hydrogen peroxides, or primary
products, are formed. Ultimately these peroxides break down, and secondary products, e.g.,
aldehydes, ketones, organic acids, and hydrocarbons, are formed.
The peroxide value (PV) test, which is one of the most common tests used to evaluate the
extent of lipid oxidation, is based on measuring peroxides.

Objective: To measure the PV or a number of food samples, and to evaluate the meaning of
the results.

Reagents:
Acetic acid (glacial)
Chloroform (CCl
4
)
15% Potassium iodide (KI)
0.01 N (0.01M) sodium thiosulfate (Na
2
S
2
O
3
)
Starch indicator 0.5 %
concentrated hydrochloric acid HCl
0.01 N (0.00167M) potassium dichromate K
2
Cr
2
O
7
(fix.)

Procedure

Determination of the titre of the sodium thiosulfate solution
Measure off 10 ml of 0.01N K
2
Cr
2
O
7
solution to a 200 ml conical flask. Add 0.5 ml
concentrated HCl and 1.0 ml 15% KI solution. Mixed exactly 1 minute and leave for 5
minutes in a dark place. Add 0.5 ml starch solution, 20 ml distilled water. Mix and titrate with
sodium thiosufate solution.
Calculate the exact normality of Na
2
S
2
O
3
knowing that in this chemical reaction 1 gram-
equivalent of K
2
Cr
2
O
7
react with 1 gram-equivalent of Na
2
S
2
O
3
(1 mole K
2
Cr
2
O
7
react with 6
moles Na
2
S
2
O
3
).

Determination of peroxide value.
Weigh 3.00 g oil (with precision of 0.001 g) into a 250 ml Erlenmeyer flask. Add 10 ml
chloroform and swirl to dissolve oil. Add 15 ml acetic acid, 1.0 ml KI solution, mix and leave
for 5 minutes (exactly !) in a dark place.
Add 30 ml distilled water and 1 ml starch inducator. Solution titrate with sodium thiosulfate
until blue colour disappears.
Do a blank determination (10 ml chloroform + 15 ml acetic acid + 1.0 ml KI + 30 ml H
2
O).
Add starch indicator (1 ml) before titrating and titrate dropwise.
Repeat the titration procedure at least 3 times. Individual results shouldnt vary more than 0,3
ml.

Calculation
Calculate the peroxide value PV for all samples from the following formula:

PV = (V
1
V
0
) x T x 1000 / m [miliequivalent available

oxygen/kg
sample ]
[meq. / kg]

where:
V
1
volume of thiosulfate solution required to titrate the sample [ml];
V
0
volume of thiosulfate solution required to titrate the blank determination [ml];
T - titre of the sodium thiosulfate solution [normality];
m mass of sample [g]


REPORT CONTENTS:
- filled up analysis report;
- description of the aim of the exercise;
- shown calculations of individual results;
- discussion of results and errors;
- comparison of the experimental data with references.