The handbook of soap manufactureSimmons, W. H. (William Herbert)
Science
The handbook of soap manufacture
Simmons, W. H. (William Herbert)
Soap
In the case of lemon oil, where the proportion of aldehydes, though of
great importance, is relatively very small, it is necessary to first
concentrate the aldehydes before determining them. For this purpose, 100
c.c. of the oil is placed in a Ladenburg fractional distillation flask,
and 90 c.c. distilled off under a pressure of not more than 40 mm., and
the residue steam distilled. The oil so obtained is separated from the
condensed water, measured, dried, and 5 c.c. assayed for aldehydes
either by the process already described, or by the following process
devised by Burgess (_Analyst_, 1904, 78):--
Five c.c. of the oil are placed in the Hirschsohn flask, about 20 c.c.
of a saturated solution of neutral sodium sulphite added, together with
a few drops of rosolic acid solution as indicator, and the flask placed
in a boiling water-bath and continually agitated. The contents of the
flask soon become red owing to the liberation of free alkali by the
combination of the aldehyde with part of the sodium sulphite, and this
coloration is just discharged by the addition of sufficient 10 per
cent. acetic-acid solution. The flask is again placed in the water-bath,
the shaking continued, and any further alkali liberated neutralised by
more acetic acid, the process being continued in this way until no
further red colour is produced. The flask is then filled with the sodium
sulphite solution, the volume of the cooled unabsorbed oil read off, and
the percentage of aldehydes calculated as before.
_Solidifying Point, or Congealing Point._--This is of some importance in
the examination of anise and fennel oils, and is also useful in the
examination of otto of rose. A suitable apparatus may be made by
obtaining three test tubes, of different sizes, which will fit one
inside the other, and fixing them together in this way through corks.
The innermost tube is then filled with the oil, and a sensitive
thermometer, similar to that described under the Titre test for fats,
suspended with its bulb completely immersed in the oil. With anise and
fennel, the oil is cooled down with constant stirring until it just
starts crystallising, when the stirring is interrupted, and the maximum
temperature to which the mercury rises noted. This is the solidifying
point.
In the case of otto of rose, the otto is continually stirred, and the
point at which the first crystal is observed is usually regarded as the
congealing point.
_Melting Point._--This is best determined by melting some of the solid
oil, or crystals, and sucking a small quantity up into a capillary tube,
which is then attached by a rubber band to the bulb of the thermometer,
immersed in a suitable bath (water, glycerine, oil, etc.) and the
temperature of the bath gradually raised until the substance in the tube
is sufficiently melted to rise to the surface, the temperature at which
this takes place being the melting point.
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