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APPARATUS
1. Grinder—either hand- or power-driven, capable of reducing soybeans to 20 mesh or finer.
2. Cotton—clean and bleached.
3. Gravity-type extraction apparatus—assembled using an extraction tube similar to the butt extraction tube in
Fig. 1. The approximate dimensions of this larger tube in mm are body o.d./i.d./length, 40/37/195; overall length,
280; stem o.d. 16. The bottom (where the main body and stem come together) of the tube should be plugged with
cotton to support the ground meal (2–2.5 cm of cotton). Support the extraction tube with a stand, clamp, or tripod
so a collection bottle can be placed under the stem of the tube. Collection bottle can be a flask or bottle 100–150
mL in size.
4. Oil sample bottle or flask of convenient size.
REAGENTS
All rights reserved. No part of this method may be reproduced or transmitted in any form or by any means without written permission of the publisher.
PROCEDURE
1. Predry 100 g of a well-mixed test sample, free of foreign matter, for 2 hr at 130 ± 3 °C and cool. Grind to 20 mesh
or finer and fill the extraction apparatus with sufficient test portion (40–50 g) to yield the required amount of oil.
2. Add 50 mL of petroleum ether or hexane and allow all of it to percolate through the test portion into a flask or
beaker. Repeat with two 25-mL portions of solvent.
3. Evaporate the solvent from the oil in a water bath under a gentle stream of clean, dry air until free from petroleum
ether or hexane.
4. Weigh 7.05 ± 0.05 g of extracted oil into a suitable size oil sample bottle or flask. Add 50–75 mL of neutral alcohol
and 1 mL of indicator. Titrate with 0.25 M NaOH, shaking vigorously until a faint pink color is obtained that
persists for at least 1 min.2
CALCULATIONS3
1. Free fatty acids, calculated as oleic, % = mL of 0.25 M alkali used.
PRECISION
TABLE 1 The average, expected between-laboratory variation (standard deviation
of reproducibility, SR) for the determination of free fatty acids in oilseeds.a
Approximate FFA value, % 0.1–1.0 1.0–2.0 2.0–3.0
NOTES
1 The compactness of the cotton plug and packing of the ground meats in the extraction apparatus should be such
that the cold percolation rate will be about 150 drops per minute and that none of the ground test portion will pass
through the cotton plug.
2 About 15 mL of petroleum ether or hexane may be added to aid in solubilizing the oil in the alcohol, if necessary.
3 The result, expressed as oleic acid, is dependent upon using the test portion weight of 7.05 g as specified. Any devia-
tion from the test portion weight of 7.05 g will yield erroneous results.
All rights reserved. No part of this method may be reproduced or transmitted in any form or by any means without written permission of the publisher.
Water-cooled
condenser
Tapered cork
stopper
Extraction tube
Sample thimble
sets here
Tapered cork
stopper
50- or 100-mL
Soxhlet flask
Tetrachloroethylene (perchloroethylene) is a colorless, volatile, nonflammable liquid stances. Perform manipulations under a properly operating fume hood. Take partic-
chlorinated hydrocarbon that will emit toxic fumes of phosgene when exposed to ular precautions, such as the use of a glove box, when toxins are in dry form, because
sunlight or flames. It is an irritant to eyes and skin. The TLV is 50 ppm in air. of their electrostatic nature and resulting tendency to disperse in working areas. Swab
accidental spills of toxin with 5% NaOCl bleach. Rinse all glassware exposed to tox-
Tetrahydrofuran is a highly flammable liquid and a dangerous fire risk. The flammable ins with 1% NaOCl bleach solution and then wash thoroughly with warm water.
limits in air are 2–11%. It is toxic by ingestion and inhalation. The TLV in air is 200
ppm. It tends to form peroxides upon storage in air.
REFERENCES
Toluene is a highly flammable liquid and a dangerous fire risk. Explosive limits in air
are 1.27–7%. It is toxic by ingestion, inhalation, and skin absorption. The TLV is Official Methods of Analysis, Association of Official Analytical Chemists, 14th edn.,
100 ppm in air. A fume hood should be used at all times when using toluene. 1984, pp. 1010–1015.
Trichloroethane is a synthetic, light-sensitive, volatile, colorless, liquid miscible with Standard Methods for the Analysis of Oils, Fats and Derivatives, 7th edn., Blackwell
many nonpolar organic solvents. It is an irritant to eyes and skin. The TLV is 350 Scientific Publications, 1987.
ppm in air.
Hawley’s Condensed Chemical Dictionary, 11th edn., revised by N. I. Sax and R. J.
Xylene is flammable and a dangerous fire risk. The TLV is 100 ppm in air. Lewis, Jr., 1987.