Thermal Analysis Application No.

UC 234
Thermal Analysis Application
Application published in METTLER TOLEDO Thermal Analysis UserCom 23

Characterization of vegetable oils by

DSC
Introduction
Differential Scanning Calorimetry (DSC)
is used to characterize very many differ-
ent types of materials in research, prod-
uct development and quality control.

The crystallization behavior of fats and

oils has been studied by DSC methods for
many years.

This article presents some interesting

DSC measurements performed on vegeta-
ble oils. Vegetable oils (or fats, depending
on their consistency) are plant constitu-
ents obtained from the seeds or fruit pulp
by pressing and/or solvent extraction fol-
lowed by evaporation of the solvent. Veg-
etable oils consist mainly of triglycerides.
Chemically, triglycerides are tri-esters,
formed by the esterification of glycerol
with three long-chain carboxylic acids
(fatty acids).
In natural oils, triglycerides contain
many different fatty acids. A natural oil
is therefore always a mixture of different
triglycerides. In addition, the oil contains
different amounts of partial glycerides
(i.e. mono- and diglycerides) and other
Figure 1. DSC curve of cold-pressed soya oil. The exothermic peaks arise through the crys-
tallization of different triglycerides in the soya oil.
constituents (e.g. phospholipids, sterols, differences between oils, for example be-
vitamins, etc.), depending on the origin tween refined and natural oils.
of the oil and the type of processing.
Experimental details
The crystallization behavior of a fat or The measurements described in this
oil is very sensitive to its composition article were performed using a DSC822e
and can easily be measured by DSC. The equipped with an IntraCooler. The sam-
DSC curve obtained from an oil sample ples were hermetically sealed in 40-µl
is characteristic of the particular oil and aluminum crucibles and cooled from
serves as a “fingerprint”. DSC is in fact 50 °C to −75 °C at 1 K/min. The sample
an excellent method for determining mass was typically 5−10 mg.
 Measurements and results
Figure 1 shows a typical DSC cooling
curve of a vegetable oil. As the oil cools,
various components crystallize out at
characteristic temperatures. These crys-
Thermal Analysis Application

tallization processes are observed on the

DSC curve as exothermic peaks.

In general, raw vegetable oils are normal-

ly unfit for direct human consumption.
The raw oils are cleaned and refined in
processes that eliminate a large number
of substances whose presence is detrimen-
tal to the taste, human health properties,
shelf life or appearance of the oil. In a
further process, the oils can be treated
to give them more desirable properties. Figure 2. Comparison of the DSC curves of cold-pressed and refined walnut oil. The exo-
thermic peaks are due to the crystallization of different triglycerides in the walnut oil.
These processes include the so-called
“hardening” or “hydrogenation” of oils,
in which the content of unsaturated fatty
acids is reduced. This increases the crys-
tallization temperature of the oil.

Figure 2 shows DSC cooling curves of

cold-pressed and refined walnut oil. Com-
parison of the two curves shows distinct
differences. The native oil (cold-pressed)
crystallizes at about −48 °C. Above this
temperature, a certain amount of crys-
tallization is visible but the correspond-
ing peaks are small. In contrast, the
refined walnut oil crystallizes at lower
temperatures and the DSC curve shows
several more pronounced peaks.
Figure 3. DSC curves of different cold-pressed (native) oils.

METTLER TOLEDO
TA Application No. UC 234 2
 As already mentioned, the crystalliza-
tion behavior of a vegetable oil depends
mainly on its chemical composition.
Vegetable oils and fats contain fatty acids
with mostly even numbers of carbon at-
Thermal Analysis Application

oms and chain lengths of 4 to 24 carbon

atoms. Quantitatively, fatty acids with
chain lengths of 14 to 18 carbon atoms
predominate.

In general, oils composed mainly of satu-

rated fatty acid triglycerides crystallize at
relatively high temperatures, whereas oils
with unsaturated fatty acid triglycerides
crystallize at relatively low temperatures.

Depending on the proportions of fatty Figure 4. DSC curves of different refined oils.

acid triglycerides present in the oils, sev-
eral crystallization peaks appear in the
DSC curve. Usually the curve exhibits
one pronounced crystallization peak (as
a rule at about −50 °C, −35 °C or 10 °C)
and one or more smaller peaks.
This is also true for the refined oils (see
Figure 4). Compared with native oils,
crystallization occurs here at slightly
lower temperatures.
Conclusions fore an extremely useful technique for
Vegetable oils exhibit characteristic crys- the quality assurance of vegetable oils.
tallization behavior that is strongly in-
fluenced by the composition of the oil.
Publishing Note:
The crystallization behavior can easily be
This application has been published in
studied by DSC methods. the METTLER TOLEDO Thermal Analysis
UserCom No. 23.
See www.mt.com/ta-usercoms
The resulting measurement curves are
used to identify unknown native and re-
fined vegetable oils and to monitor and
control refining processes. DSC is there-

Mettler-Toledo AG, Analytical www.mt.com/ta

CH-8603 Schwerzenbach, Switzerland For more information
Phone +41-44-806 77 11
Fax +41-44-806 72 60
Internet www.mt.com

Subject to technical changes

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TA Application No. UC 234 3