Practical tips: Rancimat

Tips for measuring the oxidation stability with Rancimats

The 873 Biodiesel Rancimat is one of the two Metrohm

instruments for measuring oxidation stability.

Brief Rancimat fundamentals

With the 743 Rancimat and the 873 Biodiesel Rancimat, Metrohm offers two instru-
ments for the easy and reliable determination of the oxidation stability of natural fats/
oils and biodiesel1, respectively. The method, which is also known as Rancimat meth-
od or Rancimat test, is the same in both cases. It is based on a simple reaction kinetics
principle, according to which the rate of a chemical reaction (in this case the oxidation
of the fatty acids) can be accelerated by increasing the temperature. During the deter-
mination, a stream of air is passed though the sample at a constant temperature (e.g.
110 °C as per EN 14214 for biodiesel). The oxidation products formed are transported
by the air stream to a measuring vessel where they are detected by the alteration in
conductivity of an absorption solution. In addition to the temperature, whose accuracy
and stability is guaranteed by the Rancimat, the quality and reproducibility of the results
is influenced by the measurement preparations as well as the condition of the acces-
sories used. Our practical experiences with handling Rancimats have been collected
and are presented below.

1 Before the determination

1.1 Removing foreign bodies from the reaction vessel
Foreign bodies in the reaction vessel could catalyze reactions in the sample and lead
to poorly reproducible results. Remove all foreign bodies, such as residual packaging
material, from the reaction vessel with the help of a vigorous gas stream (preferably
nitrogen).

1.2 Weighing out the sample

The sample is weighed out directly into the reaction vessel (article number: 6.1429.040
or 6.1429.050). Care must be taken that the maximum filling height does not exceed
3.5 cm. An error of ±10% in weighing out the sample has no influence on the final
result.

Diagram showing the permitted sample

amount in the reaction vessel. The maxi-
mum sample volume is approx. 9 mL. For
larger volumes the method parameter «Del-
ta T» (parameter for correcting the temper-
Insulation ature difference between heating block and
Maximum sample) must be adjusted.
sample level

�
The minimum sample volume is approx.
2.5 mL. The sample volume must be se-
Minimum lected so that the air tube is immersed in
Heating
sample level the sample.
block
__________________________
1
Biodiesel is a fuel obtained from natural oils such as, for example, rapeseed oil or soybean oil.

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Practical tips: Rancimat

1.3 Checking the reaction vessel cover

The green reaction vessel cover (article number: 6.2753.100) must seal the reac-
tion vessel hermetically. If this is no longer the case, the cover must be replaced.
Leaking reaction vessel covers produce incorrect and irreproducible results.

1.4 Positioning the air tube in the reaction vessel

The reproducibility of the results can be improved by always installing the air tube
(article number: 6.2418.100 or 6.2418.130) in the same position inside the reac-
tion vessel.

With foam barrier

correct

If the foam barrier (article number: 6.1451.010) is

used, the air tube will automatically be positioned
correctly. The foam barrier must be fixed in the
upper half of the reaction vessel as it could melt if
located within the heating block.

�
Without foam barrier
correct incorrect

If no foam barrier is used, the air tube must touch

the glass wall at the bottom of the reaction vessel.

� �
1.5 Absorption solution in the measuring vessel
Deionized water is used as the absorption solution of the conductivity cell. At the
start of the measurement, the specific conductivity of the water in the measuring
vessel should not exceed a value of 5 µS/cm.

1.6 Positioning the air supply tubing

The PTFE tubing (article number: 6.1819.080) that leads the air stream from the
reaction vessel to the absorption solution must be positioned such as to avoid
bubbles reaching directly the electrodes of the conductivity cell. Air bubbles at the
electrodes produce noisy measuring curves that are difficult to evaluate.

correct air supply incorrect air supply

� �
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 Practical tips: Rancimat

2 Starting the determination

• The temperature of the heating block defined in the method must have been
reached and must be stable before the reaction vessel is inserted.
• When all the air supply tubing has been connected and the pump switched on,
a uniform gas flow must be recognizable in both the sample and the measuring
solution.
• Data recording with the Rancimat software must be started immediately after
the sample has been inserted in the heating block.

3 After the determination

3.1 Switching off the instrument
If the tubing connections for the air supply are left connected and if the gas flow and
heating are switched off simultaneously then, on rare occasions, the sample could be
drawn off into the air supply. To avoid this and for safety reasons, you should first dis-
connect the tubing between the instrument and the reaction vessel before you switch
off the air pump or the instrument itself.

3.2 Cleaning the accessories

Hot water, detergent and a brush is used to remove larger contaminants from the
reaction vessel cover, transfer tubing, measuring vessels and conductivity cells
first. These items are then thoroughly cleaned using a brush and a solvent (e.g.
acetone, 2-propanol or a 1:1 mixture of acetone and ethanol). Finally they must be
carefully rinsed with deionized water.
• Reaction vessels
We recommend that the reaction vessels (article number: 6.1429.040 or
6.1429.050) and their gas inlet tubes (article number: 6.2418.100 or 6.2418.130)
are used only once. Insufficient cleaning or glass damage caused by cleaning
causes irreproducible results.
• Polycarbonate measuring vessels
Polycarbonate measuring vessels (article number: 6.1428.100) are not resis-
tant to acetone. In this case we recommend the use of ethanol or 2-propanol as
cleaning solvent. Measuring vessels made of glass (article number: 6.1428.030)
can be cleaned as described above.
• Conductivity electrode
For easier cleaning, the protective ring of the conductivity electrode can be re-
moved. However, do not forget to place it back when cleaning has been com-
pleted.

3.3 Heating the reaction vessel cover and transfer tubing

Both the material of the reaction vessel cover and the transfer tubing absorb re-
action products during the measurement. In order to avoid carryover to the next
measurement, it is important that these accessories are kept at 80 °C for at least 2
hours in a drying oven.
We hope that these easy-to-follow tips help you to save time and trouble in your
daily Rancimat work. We wish you successful determinations!

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