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]
Fig. 85.—Apparatus
for Determining
Crystallizing Point.