The Extraction

Procedure
 — 2 —

To perform an extraction, for example, using a Soxhlet extraction apparatus, the

following equipment, accessories and expendables are needed:
Accessories and Expendables
Stock Number:
Evaporating dish, 70 mm diam., glass QL9000113
Beaker, 100 ml VG1121116241
Desiccator, DN 150 (for a single extraction) QL9042031
with desiccator plate QL9042514
Desiccator, DN 300 (for multiple extractions) QL9042047
with desiccator plate QL9042528
Homogenizer with stand, clamps and accessories QL9571195
Analytical balance with 0,001 accuracy, for example QL6250429
Plastic spatula / spoon combination 80596
Drying oven
Extraction thimbles for the 100 ml Soxhlet VG804841034
Boiling chips VG804830700
Silica gel, 1 kg CBKIESELGEL1L
Cotton, 400 g QL9413151
Extraction solvent, for example
Petroleum ether; boiling fraction 40 – 60 °C
Sodium sulfate, anhydrous
Sand
Equipment
Stock No. Model No. of Control of Time-Temp.
samples heating power Control
804800522 KEX 100 F 1 X –
804880023 In-line heating 4 Individually for –
unit R 104 S each sample

804880022 In-line heating 6 Individually for –

unit R 106 S each sample

Heating block X
system
804850020 DET
804850025 (DBAS +
DFE 100)
 — 3 —

Preparation for the

Extraction

Place 3 or 4 boiling chips into the

solvent vessel (e.g round bottom
flask or cylindrical flask).

Dry the solvent vessel in a drying

oven to constant weight
(about 1 hour) at 103±2 °C

Fill the silica gel into the desiccator

and insert the desiccator plate..
Allow the desiccator to cool to
room temperature
(about 30 minutes).
 — 4 —

Weigh the solvent vessel

containing the boiling chips to
an accuracy of ±1 mg.

Sample Preparation

Homogenize or grind the

sample.
 — 5 —

Ground
sample

dry moist liquid

0.000 ON
OFF
TARE
0.000 ON
OFF
TARE

weigh weigh weigh

dry mix

wipe

cover

extract drain
 — 6 —

Dry Samples

Weigh the ground dry sample into the

extraction thimble.
For example, weigh out 6.6 g with an
expected fat content of at most 2 g.

Moist Samples

Moist samples must be dried for

2 – 3 hours at 103±2 °C in a drying
oven after having been weighed in
the extraction thimbles.

Liquid Samples Containing

Water Content

Weigh the liquid sample into an

evaporating dish
 — 7 —

Mix the liquid sample with sand

and anhydrous sodium sulfate.

Use a cotton swab, which has

been moistened with extraction
solvent, to wipe the sample into
the extraction thimble.

Extraction

Close the extraction thimble with a

fat-free cotton wad
Insert the thimble into the Soxhlet
extractor
If the Soxhlet extractor has a spigot for
solvent draining, close the spigot.
 — 8 —

Fill the solvent into the solvent vessel.

Extract at a temperature of 110-130 °C
for 20 – 30 extraction cycles
(4 – 6 hours), depending on the nature
of the sample and the solvent
employed.
 — 9 —

Drain the solvent into a suitable container

by opening the spigot on the Soxhlet
extractor.
Continue to heat the solvent vessel until
all of the solvent has been evaporated
and condensed in the Soxhlet extractor
(spigot closed). Care must be taken not to
heat the fat residue to decomposition.
The thus recovered solvent may be
reused for subsequent extractions.
 — 10 —

Place the vessel containing

the fat residue in a drying
oven at 103±2 °C and heat to
constant weight (indicating
evaporation of all solvent.
After every completion of the
solvent evaporation step, air
the drying oven out by
leaving the door open.
Observe carefully all safety
guidance of the oven
manufacturer.

Allow the vessels

containing the fat to
cool to room
temperature (about 30
minutes).
 — 11 —

Weigh the vessel

containing the boiling chip
and fat residue.

Compute the fat content according to the

following formula:

m 2 − m1
F [%] = • 100 where
E
m1 is the weight of the dry empty vessel, in
grams, including the boiling chips,
m2 is the weight of the vessel, in grams,
containing the boiling chips and fat residue
after evaporation of the solvent and

E is the sample weight in grams.

behr Labor-Technik GmbH • Spangerstraße 8 • D – 40599 Düsseldorf/Germany
Tel. +49 (0)211 748 47 17 • Fax: +49 (0)211 748 47 48 • email: j.behr@behr-labor.com • http://www.behr-labor.com