When the temperature of the alcohol-water mixture rises to about
6° below the melting point, the disk of fat begins to shrivel, and
gradually rolls up into an irregular mass.
The thermometer is now lowered until the fat particle is even with the
center of the bulb. The bulb of the thermometer should be small, so as
to indicate only the temperature of the mixture near the fat. A gentle
rotatory movement from time to time should be given to the thermometer
bulb. The rise of temperature should be so regulated that the last
2° of increment require about ten minutes. The mass of fat gradually
approaches the form of a sphere, and when it is sensibly so the reading
of the thermometer is to be made. As soon as the temperature is taken
the test tube is removed from the bath and placed again in the cooler.
A second tube, containing alcohol and water, is at once placed in the
bath. The test tube (ice water having been used as a cooler) is of
low enough temperature to cool the bath sufficiently. After the first
determination, which should be only a trial, the temperature of the
bath should be so regulated as to reach a maximum of about 1°.5 above
the melting point of the fat under examination.
The edge of the disk should not be allowed to touch the sides of the
tube. This accident rarely happens, but in case it should take place,
and the disk adhere to the sides of the tube, a new trial should be
made.
Triplicate determinations should be made, and the second and third
results should show a near agreement.
_Example._—Melting point of sample of butter:
Degrees.
First trial 33.15
Second trial 33.05
Third trial 33.00
The fatty acids, being soluble in alcohol, cannot be treated as the
ordinary glycerids. But even those glycerids which are slightly soluble
in alcohol may be subjected to the above treatment without fear of
experiencing any grave disturbance of the fusing points.
=293. Solidifying Point.=—The temperature at which a fat shows
incipient solidification is usually lower than the point of fusion.
The same difficulties are encountered in determining the temperature
of solidification as are presented in observing the true melting
point. The passage from a transparent liquid to an opaque solid is
gradual, showing all the phases of turbidity from beginning opalescence
to complete opacity. The best the analyst can do is to determine,
as accurately as possible, the temperature at which the more solid
glycerids of the mixture begin to form definite crystals. This point is
affected to a marked degree by the element of time. A fat cooled just
below its melting point will become solid after hours, or days, whereas
it could be quickly cooled far below that temperature and still be
limpid.
The methods of observation are the same for the glycerids and fatty
acids, and the general process of determination is sufficiently set
forth in the following description of the method as used in this
laboratory.[246]
Public-domain text, read in full here on John Shaqi.
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