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
samples
Control of
heating power
Time-Temp.
Control
804800522 KEX 100 F 1 X
804880023 In-line heating
unit R 104 S
4 Individually for
each sample

804880022 In-line heating

unit R 106 S
6 Individually for
each sample

804850020
804850025
Heating block
system
DET
(DBAS +
DFE 100)
X
3
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 1032 C
Fill the silica gel into the desiccator
and insert the desiccator plate..
Allow the desiccator to cool to
room temperature
(about 30 minutes).
Preparation for the
Extraction
4
Weigh the solvent vessel
containing the boiling chips to
an accuracy of 1 mg.
Homogenize or grind the
sample.
Sample Preparation
5
ON TARE OFF 0.000
ON TARE OFF 0.000
Ground
sample
dry moist liquid
weigh weigh
dry
mix
wipe
cover
extract drain
weigh
6
Moist samples must be dried for
2 3 hours at 1032 C in a drying
oven after having been weighed in
the extraction thimbles.
Weigh the liquid sample into an
evaporating dish
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.
Dry Samples
Moist Samples
Liquid Samples Containing
Water Content
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.
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.
Extraction
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 1032 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:
[ ] 100 %
1 2

=
E
m m
F where
m
1
is the weight of the dry empty vessel, in
grams, including the boiling chips,
m
2
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 Spangerstrae 8 D 40599 Dsseldorf/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