SAMPLING AND ANALYSIS OF OILSEED BY-PRODUCTS

AOCS Official Method Ba 3-38

Reapproved 2009

Oil
DEFINITION
This method determines the substances extracted by petroleum ether under the conditions of the test.
SCOPE
Applicable to cottonseed meats, and cake and meal from cottonseed, soybeans, peanuts, and flaxseed.

APPARATUS
1. Butt-type extraction apparatus—assembled exactly as indicated in Apparatus, 1 of AOCS Official Method Aa 4-38. See
Figure 1 below.
2. Filter paper—150 mm; S & S no. 597, Whatman no. 2, Reeve Angel no. 211, or equivalent.
3. Absorbent cotton—free of petroleum ether extractables.
4. Porcelain mortar and pestle—The mortar must be at least 4 in. i.d. at the top. The pestle handle must be large enough to
afford a firm hand grip. The inner surface of the mortar is kept rough by occasionally grinding with sand.
5. Sieve—US no. 20.
6. Sieve—US no. 30.
7. Laboratory mill—suitable for grinding the samples to a maximum particle size of 0.850 mm (US no. 20 sieve); except for
linseed meal, for which the samples are ground to a maximum particle size of 0.600 mm (US no. 30 sieve).

REAGENTS
1. Petroleum ether—AOCS Specification H 2-41 (see Notes, Caution).

PREPARATION OF TEST SAMPLE

1. Grind the 100-g portion from AOCS Official Method Ba 2a-38, Preparation of Test Sample, through the laboratory mill
to a uniform fineness (maximum particle size of 0.850 mm, 20 mesh), except for linseed meal (maximum particle size of
0.600 mm, 30 mesh). Immediately return to an airtight container. Oil, ground moisture, and protein nitrogen are deter-
mined on this portion.

PROCEDURE
1. Meal and ground cake or pellets—
(a) Weigh 5 g of the ground test sample into a filter paper and enclose in a second filter paper, folded in such a fashion as
to prevent escape of the meal (see Fig. 2). The second paper is left open at the top like a thimble. A piece of absorbent
cotton may be placed in the top of the thimble to distribute the solvent as it drops on the test portion.
(b) Place wrapped test portion in the Butt extraction tube and assemble the apparatus as shown in Figure 1. Put about
25 mL of petroleum ether into the tared extraction flask before attaching to the tube.
(c) Heat in a water bath or on an electric hot plate at such a rate that the solvent will drop from the condenser on the center
of the thimble at the rate of at least 150 drops/min.
(d) Keep the volume of solvent fairly constant by adding enough to make up for any that may be lost due to evaporation.
Continue extraction for 3 hr.
(e) Cool and disconnect the extraction flask. Evaporate the petroleum ether on a steam bath or in a water bath until no
odor of solvent remains. A gentle stream of clean, dry nitrogen may be used to facilitate removal of the solvent. Cool to
room temperature, carefully remove any moisture or dirt from the outside of the flask and weigh. Repeat heating until
constant weight is obtained.
(f ) Determine the moisture in the ground test sample as directed in AOCS Official Method Ba 2a-38.
2. Cottonseed meats—
(a) Weigh accurately about 2 g of the ground test sample and proceed as directed in Procedure, 1, (a) above, continuing the
extraction for 2 hr only.
(b) Remove the thimble from the Butt tube, allow the solvent to evaporate from the filter paper and test portion at room
temperature. Then carefully transfer the test portion to the mortar so there will be no loss. Grind the test portion in the
mortar with the pestle for at least 1 min, or with at least 100 vigorous strokes. Use no abrasive.
(c) Return the reground test portion to the same filter paper and continue the extraction as before for an additional 2 hr.
From here on, proceed as directed in Procedure 1, (d), (e), and (f ).

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 SAMPLING AND ANALYSIS OF OILSEED BY-PRODUCTS
Ba 3-38 • Oil

CALCULATIONS
mass, g of oil
1. Oil, % =   ×  100
mass, g of test portion
2. The percentage oil may be calculated to any desired moisture basis with the following formula:
F(100 − % moisture desired)
Oil, desired moisture basis, % =   ×  100
100 − % moisture in test portion analyzed
Where—
F = percent oil in test portion analyzed

NOTES
Caution
Petroleum ether is extremely flammable. Avoid static electricity. The explosive limits in air are 1–6%. A fume hood should be used
at all times when using petroleum ether.

Water-cooled
condenser

Tapered cork
stopper

Butt tube

Sample thimble
sets here

Tapered cork
stopper

50 or 100 mL
Soxhlet flask

Figure 1. Butt-type extraction apparatus.

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 SAMPLING AND ANALYSIS OF OILSEED BY-PRODUCTS
Ba 3-38 • Oil

Test sample Fold here

Filter paper

15 cm

ca. 5 cm 3

ca. 5 cm
Fold here
1 2

Fold here

ca. 5 cm

4 5 6

Timble ca. 3 cm
Filter paper
ca. 5 cm
15 cm
ca. 2 cm

Sample
envelope ca. 5 cm
Sample envelope
7 8 9

Place in Butt tube

Fold here with this end up

11 Thimble containing
test sample in
sample envelope

10 12

Figure 2. For oil extraction, fold filter paper in the sequence shown, steps 1 through 12.

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