AOAC 965.33 Peroxide Value

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41.1.16 and swirl to dissolve. Add 0.

5 mL saturated KI solution, (b), from


AOAC Official Method 965.33 Mohr pipet, let stand with occasional shaking 1 min, and add 30 mL
Peroxide Value of Oils and Fats H2O. Slowly titrate with 0.1M Na2S2O3 with vigorous shaking until
Titration Method yellow is almost gone. Add ca 0.5 mL 1% starch solution, and
First Action 1965 continue titration, shaking vigorously to release all I2 from CHCl3
Final Action 1969
layer, until blue just disappears. If <0.5 mL 0.1M Na2S2O3 is used,
AOCS–AOAC Method
repeat determination with 0.01M Na2S2O3.

(Note: Conduct analysis in diffuse daylight or in artificial light Conduct blank determination daily (must be ≤0.1 mL 0.1M
shielded from direct light source.) Na2S2O3). Subtract from test portion titration.
A. Reagents
(a) Ace tic acid–chloroform so lu tion.—Mix 3 vol umes Peroxide value (milliequivalent peroxide/kg oil or fat) = S × M ×
CH3COOH with 2 volumes CHCl3, USP. 1000/g test portion, where S = mL Na2S2O3 (blank corrected) and M
(b) Potassium iodide solution, saturated.—Dissolve excess KI = molarity Na2S2O3 solution.
in freshly boiled H2O. Excess solid must remain. Store in dark. Test
daily by adding 0.5 mL to 30 mL CH3COOH–CHCl3, (a); then add (b) Margarine.—Melt fat by heating with constant stirring on hot
2 drops 1% starch solution, (mix ca 1 g soluble starch with enough plate at low heat, or heat in air oven at 60°–70°C. (Avoid excessive
cold water to make thin paste, add 100 mL boiling H2O, and boil ca heat and long exposure >40°C.) When completely melted, hold in
1 min while stirring). If solution turns blue, requiring >1 drop 0.1M warm place until aqueous portion and most of solids have settled.
Na2S2O3 to discharge color, prepare fresh solution. Decant oil into clean beaker and filter through Whatman No. 4, or
(c) Sodium thiosulfate standard solutions.—0.1 and 0.01M.
equivalent paper. Do not reheat unless necessary to obtain clear
Prepare and standardize as in 942.27 (see A.1.13). For 0.01M, dilute
filtrate. Proceed as in (a).
0.1M with freshly boiled and cooled H2O.
B. Determination References: J. Am. Oil Chem. Soc. 26, 345(1949).
(a) Fats and oils.—Weigh 5.00 ± 0.05 g test portion into 250 mL AOCS Method Cd 8–53.
glass-stoppered Erlenmeyer. Add 30 mL CH3COOH–CHCl3, (a), JAOAC 48, 175(1965).

 2005 AOAC INTERNATIONAL

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