AOCS OxiraneOxygen

SAMPLING AND ANALYSIS OF COMMERCIAL FATS AND OILS
AOCS Official Method Cd 9-57

Reapproved 1997
Oxirane Oxygen
DEFINITION
This method determines oxirane oxygen which is the oxygen contained in the following grouping.
Under the prescribed conditions of this test method, the oxygen is titrated directly with hydrogen bro-
mide in acetic acid.
SCOPE
Applicable to epoxidized fatty materials and epoxy compounds in general (see Notes, 1).
APPARATUS (c) Standardization—Accurately weigh about 0.4 ±

1. Burette assembly—with either gravity feed or reservoir 0.0001 g of potassium acid phthalate into a 50-mL
bottle. The assembly should be an enclosed system for Erlenmeyer flask. Dissolve in 10 mL of glacial
titration to avoid the loss of hydrogen bromide. Attach acetic acid, warming slightly to dissolve. Titrate the
the titration flask to the burette tip with a one-hole solution at room temperat u re with hy d roge n
ru bber stopper. The hole in the stopper should be bromide in acetic acid, using no more than 0.1 mL
formed so the burette tip fits snugly in the stopper with (5 drops from a fine dropping pipet) of crystal violet
a small side opening to permit air to escape from the indicator. The standardization should be performed
flask during titration. in duplicate with a difference not exceeding 0.0004
2. Erlenmeyer flasks—50 mL. N. The HBr must be standardized on the same day
3. A magnetic stirre r — a ny suitable type with ro u n d that samples are analyzed (see Notes, 2).
magnetic stirring bars covered with Teflon™ protective mass of potassium acid phthalate, g
coating, or equivalent. Normality of HBr =
0.2042 × mL HBr solution
REAGENTS PROCEDURE
1. Glacial acetic acid—reagent grade, free of acetic anhy- 1. Weigh 0.3 – 0.5 ± 0.0001 g of sample into a 50-mL
dride. Erlenmeyer flask. Dissolve the sample in 10 mL of
2. Hydrogen bromide gas—anhydrous, available in small glacial acetic acid or chlorobenzene (in the case of
cylinders, or 30–32% hydrogen bromide in acetic acid epoxy resins use chlorobenzene). Add the coated stir-
(see Notes, Caution). ring bar and no more than 0.1 mL (5 drops from a fine
3. Crystal violet—gentian violet. dropping pipet) of crystal violet indicator.
4. Potassium acid phthalate—primary standard grade, 2. Place the rubber stopper in position and lower the tip of
dried for 2 hr at 120°C and allowed to cool to room the burette until it will discharge just above the surface
temperature in an efficient desiccator prior to use. of the solution. This is important to avoid loss of HBr.
5. Chlorobenzene—reagent grade (see Notes, Caution). 3. Stir and titrate the sample (rapidly at first) with the 0.1
N HBr solution to a blue-green end point that persists
SOLUTIONS for 30 sec. Control the rate of the magnetic stirrer to
1. Crystal violet indicator solution—prepared by dissolv- avoid splashing.
ing 0.1 g of crystal violet (gentian violet) in 100 mL of
glacial acetic acid. CALCULATIONS
2. Hydrogen bromide (HBr)—0.1 N solution in acetic mL HBr to titrate sample × N × 1.60
Oxirane oxygen, % =
acid, prepared by one of the following procedures: mass of sample, g
(a) B u bble hy d rogen bromide gas through glacial Where—
acetic acid to ap p rox i m at e ly 0.1 N. A suitabl e N = normality of HBr solution
balance should be used to estimate the amount of
hydrogen bromide added. PRECISION
Note—This procedure should be carried out The average variance of components calculated from the
in a properly operating fume hood. collaborative study data obtained by the AOCS Technical
(b) Dilute 30–32% (ap p rox i m at e ly 4 N) hy d roge n Committee indicate the following 95% probability limits—
bromide in acetic acid with glacial acetic acid to 1. The difference between duplicate determinations made
approximately 0.1 N. within one laboratory should not exceed 0.08.
Page 1 of 2
SAMPLING AND ANALYSIS OF COMMERCIAL FATS AND OILS
Cd 9-57 • Oxirane Oxygen
2. The difference between the average of duplicate deter- TLV in air is 75 ppm. Use a properly operating fume hood
minations made in different laboratories should not when working with this solvent.
exceed 0.19.
NUMBERED NOTES
NOTES 1. This method is not applicable to oils containing α- and
Caution β- u n s at u rated ketones, cy cl o p ropenes, conjugat e d
Hydrogen bromide gas and hydrogen bromide are toxic by dieneols, oxidized fats and soaps.
inhalation and strong irritants to eyes and skin. Use a properly 2. Long standing has a deleterious effect on hydrogen
operating fume hood when working with these compounds. bromide solutions and should be avoided. The hydro-
Chlorobenzene is a moderate fire risk. Explosive limits gen bromide solution should be standardized each time
in air are 1.8–9.6%. Avoid inhalation and skin contact. The prior to use.
Page 2 of 2

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SAMPLING AND ANALYSIS OF COMMERCIAL FATS AND OILS

AOCS Official Method Cd 9-57

APPARATUS (c) Standardization—Accurately weigh about 0.4 ±

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