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Objective
To determine the peroxide value of fats and oils, in terms of meq peroxide per
1000 g of sample. The method is applicable to all normal fats and oils including
margarine. It is highly empirical, and any variation in procedure may result in
variation in results. This method is equivalent to Official Method Cd 8-53 of the
American Oil Chemists Society (AOCS).
Apparatus
1. Pipet, Mohr, measuring type, 1-ml capacity.
2. Erlenmeyer flasks, glass-stoppered, 250-ml.
Reagents
1. Acetic acid-chloroform solution. Caution. See Note 1. Mix 3 parts by
volume glacial acetic acid, reagent grade, with 2 parts by volume chloroform,
U.S. Pharmacopeia grade. See Note 2.
2. KI solution, saturated solution of KI, ACS grade, in recently boiled distilled
water. Make sure solution remains saturated as indicated by presence of undis-
solved crystals. Store in dark. Test daily by adding 2 drops starch solution (see
Note 3) to 0.5 ml KI solution in 30 ml acetic acid-chloroform solution. If blue
color is formed that requires more than 1 drop 0.1N sodium thiosulfate solution
to discharge, discard KI solution and prepare fresh solution.
3. Sodium thiosulfate solution, 0.1N, accurately standardized.
4. Sodium thiosulfate solution, 0.01N, accurately standardized. This solution
may be prepared by accurately pipetting 100 ml 0.1N solution into 1000-ml
volumetric flask and diluting to volume with recently boiled distilled water.
5. Starch indicator solution, 1.0% of soluble starch in distilled water.
Calculation
( S B )( N )( 1000)
Peroxide value as milliequivalents peroxide per 1000 g sample =
weight of sample
where B = titration of blank, S = titration of sample, N = normality of Na2S2O3
solution.
Notes
1. Chloroform is a known carcinogen. It is toxic by inhalation and has
anesthetic properties. Avoid contact with the skin. Prolonged inhalation or
ingestion can lead to liver and kidney damage and may be fatal. It is nonflamma-
ble but will burn on prolonged exposure to flame or high temperature. The
threshold limit value (TLV) is 10 ppm in air. A fume hood should be used at all
times when using chloroform.
Acetic acid in the pure state is moderately toxic by ingestion and inhalation. It
is a strong irritant to skin and tissue. The TLV in air is 10 ppm.
2. Isooctane has been proposed as a replacement for chloroform in this
method. The method using isooctane is now available as AOCS Official Method
Cd 8b-90. The acetic acid-chloroform version of the method is intended for
deletion by AOCS.
3. Potato starch for iodometry is recommended, because this starch produces
a deep blue color in the presence of the iodonium ion. Soluble starch is not
recommended because a consistent deep blue color may not be developed when
some soluble starches interact with the iodonium ion.
Special Properties of Fats, AACC Method 58-16
Oils, and Shortenings Page 3 of 3
References
1. American Oil Chemists Society. 1998. Official Methods and Recommended Practices, 4th ed.
Method Cc 8-53. The Society, Champaign, IL.
2. AOAC International. 1995. Official Methods of Analysis of AOAC International, 16th ed.
Method 965.33. The Association, Gaithersburg, MD.