Determination of peroxide value

Aim

To estimate the amount of peroxide value in given oil sample

Principle

Peroxide value is a measure of the peroxide content in the oil. The peroxide present in oil is
titrated against thiosulphate in the presence of potassium iodide. Starch is used as indicator.

Materials and chemicals

0.01 N Potassium dichromate

Solvent mixture 3:1 (Mix 3 volmes of glacial acetic acid with 1 volumes CHCl3)

5% KI solution (5 g of KI in 100 mL of distilled water)

0.01N sodium thiosulphate solution

1% starch indicator

Procedure

Titration 1: Standardization of sodium thiosulphate (Na2S2O3)

Weigh accurately 1.2 g of K2CrO7. Transfer into 250 mL standard flask. Dissolve in
distilled water, 5 mL of dilute H2SO4 is added before making it. The solution is made up to mark,
solution of uniform concentration 20 mL of solution is pippetted out, then transferred into a clean
conical flask. 5 mL of concentrated HCl is first added, followed by 10 mL of 5% KI solution, the
liberated iodine is titrated against Na2S2O3 taken in burette. When a light brown color solution is
attained, 0.5 mL of 1 % starch solution is added, titration is continued. The end point is change
of dark blue solution to pale green. The titration is repeated to get concordant value.

Titration 2: Determination of peroxide value

Weigh accurately 5 g of oil in a 250 mL conical flask, 50 mL of solvent mixture. Boil the
flask until the oil is completely dissolved. Add 0.5 mL of saturated KI solution. Make the solution
stand for 1 min. Overall shaking, then add 30 mL of distilled water. Titrate the liberated iodine
with Na2S2O3 with continous, vigourous shaking. When light yellow color appears, add 1 mL of
starch, continue till blue color disappears. Titration is repeated for concordance.

Result:

The peroxide value of the given oil is _______ milli equivalent/litre of oil.
 Titration 1: Standardization of sodium thiosulphate

Standardization of 0.01 N sodium thiosulphate Vs 0.01 N Potassium dichromate

Indicator: Starch 1%

End point: Dark blue to pale green

S.No Volume of conical flask Burette Reading(ml) Concordant

solution (ml) Initial Final value
1 20 ml Potassium dichromate
+ 5 ml of conc. HCl + 10 ml
of 5%KI mix well. Add 0.5
ml of starch indicator
2 20 ml Potassium dichromate
+ 5 ml of conc. HCl + 10 ml
of 5%KI mix well. Add 0.5
ml of starch indicator

Volume of K2CrO7, V1 =

Normality of K2CrO7 N1 =

Volume of Na2S2O3, V2 =

Normality of Na2S2O3, N2 =

V1 N1 = V2N2

N2= (V1 N1)/ V2

N2=

N2=
Titration 2: Determination of peroxide value

S.No Volume of conical flask Burette Reading(ml) Concordant

solution (ml) Initial Final value
1 5 g of oil + 30 ml of solvent
mixture + 0.5 ml of
saturated KI + 25 ml od
distilled water

2 5 g of oil + 30 ml of solvent
mixture + 0.5 ml of
saturated KI + 25 ml od
distilled water

Calculation

Weight of oil =

Volume of Na2S2O3 =

𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑁𝑎2𝑆2𝑂3×𝑁2
Peroxide Value =
𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑡ℎ𝑒 𝑠𝑎𝑚𝑝𝑙𝑒×1000

= mill equivalent / liters of oil