Solid–Liquid Extraction
There are instances in which the analyte needs to be extracted from a solid material
sample rather than a liquid As in the above discussion for liquid samples, such an
experiment is performed either because it is not possible or necessary to dissolve the
entire sample or because it is undesirable to do so because of interferences that may also
be present. In these cases, the weighed solid sample, preferably finely divided, is brought
into contact with the extracting liquid in an appropriate container (not a separatory
funnel) and usually shaken or stirred for a period of time, sometimes at an elevated
temperature, such that the analyte species is removed from the sample and dissolved in
theliquid. The time required for this shaking is determined by the rate of the dissolving. A
separatory funnel is not used since two liquid phases are not present, but rather a liquid
and a solid phase. A simple beaker, flask, or test tube usually suffices. Following the
extraction, the undissolved solid material is then filtered out and the filtrate analyzed.
Examples of this would be soil samples to be analyzed for metals, such as potassium or
iron, and polymer film or insulation samples to be analyzed for formaldehyde residue.
The extracting liquid may or may notbe aqueous. Soil samples being analyzed for metals,
for example, utilize aqueous solutions of appropriate. inorganic compounds, sometimes
acids, while soil samples, or the polymer films or insulation samples referred to above,
being analyzed for organic compounds utilize organic solvents for the extraction. As with
the liquid–liquid examples, the extract is then analyzed by whatever analytical technique
is appropriate— atomic absorption for metals and spectrophotometry or gas or liquid
chromatography for organics. Methods for increasing the concentration of the analyte in
the extract may also be required, especially for organics. It may be desirable to try to
keep the sample exposed to fresh extracting solvent as much as possible during the
extraction in order to maximize the transfer to the liquid phase. This may be
accomplished by pouring off the filtrate and reintroducing fresh solvent periodically
during the extraction and then combining the solvent extracts at the end. There is a
special technique and apparatus, however, that have been developed, called the Soxhlet
extraction , which accomplish this automatically
The Soxhlet apparatus is shown in above. The extracting solvent is placed in the flask at
the bottom, while the weighed solid sample is placed in the solvent-permeable thimble in
the compartment directly above the flask. A condenser is situated directly above the
thimble. The thimble compartment is a sort of cup that fills with solvent when the solvent
in the flask is boiled, evaporated, and condensed on the condenser. The sample is thus
exposed to freshly distilled solvent as the cup fills. When the cup is full, the glass tube
next to the cup is also full, and when it (the tube) begins to overflow, the entire contents
of the cup are siphoned back to the lower chamber and the process repeated. The
advantages of such an apparatus are:
1) fresh solvent is continuously in contact with the sample (without having to introduce
more solvent, which would dilute the extract), and
2) the experiment takes place unattended and can conveniently occur overnight if desired.
