The melting point determined by the capillary method is the temperature at which the last solid particle of a compact column of a substance in a tube passes into the liquid phase.
Melting Point Determination Procedure
Method I
Unless otherwise prescribed, dry the finely powdered substance in vacuo and over anhydrous silica gel R for 24 h. Introduce a sufficient quantity into a capillary tube to give a compact column 4 mm to 6 mm in height. Raise the temperature of the bath to about 10 °C below the presumed melting point and then adjust the rate of heating to about 1 °C/min. When the temperature is 5 °C below the presumed melting point, correctly introduce the capillary tube into the instrument. For the apparatus described above, immerse the capillary tube so that the closed end is near the centre of the bulb of the thermometer, the immersion mark of which is at the level of the surface of the liquid. Record the temperature at which the last particle passes into the liquid phase.
Method V
Heat the block at a suitably rapid rate to a temperature about 10 °C below the presumed melting temperature, then adjust the heating rate to about 1 °C/min. At regular intervals drop a few particles of powdered and, where appropriate, dried substance, prepared as for the capillary tube method, onto the block in the vicinity of the thermometer bulb, cleaning the surface after each test. Record the temperature t1 at which the substance melts instantaneously for the first time in contact with the metal. Stop the heating. During cooling drop a few particles of the substance at regular intervals on the block, cleaning the surface after each test. Record the temperature t2 at which the substance ceases to melt instantaneously when it comes in contact with the metal.
The instantaneous melting point is calculated using the following expression:
إرسال تعليق