Thiele melting point apparatus

Fig. 3. Thiele melting point apparatus A, groove for pressure equalization B, flame.

Apparatus Thiele melting-point apparatus, micro boiling-point apparatus, and a Bunsen burner or microburner. 

The melting point may be determined using either a commercial melting point apparatus or a Thiele tube. 

There are two principal types of melting-point apparatus available the Thiele tube and commercially available, electrically heated instruments. The Thiele tube, shown in Figure 9.3, is the simpler device and was once widely used. It is a glass tube designed to contain a heating oil (mineral oil or silicone oil) and a thermometer to which a capillary tube containing the sample is attached. For best results... 

Place the microscale assembly in a standard melting-point apparatus (or a Thiele tube if an electrical apparatus is not available) to determine the boiling point. Heating is continued until a rapid and continuous stream of bubbles emerges from the inverted capillary. At this point, stop heating. Soon, the stream of bubbles slows down and stops. When the bubbles stop, the liquid enters the capillary tube. The moment at which the liquid enters the capillary tube corresponds to the boiling point of fhe liquid, and fhe femperafure is recorded. 

A simple type of melting-point apparatus is the Thiele tube, shown in Figure 2.17a. This tube is shaped such that the heat applied to a heating liquid in the sidearm by a burner is distributed evenly to all parts of the vessel by convection currents, so... 

Some kinds of melting-point apparatus, such as the Thiele tube, use mineral or silicone oils as the heat transfer medium.These oils may not be heated safely if they are contaminated with even a few drops of water. Heating these oils above 100 °C may produce splattering of hot oil as the water turns to steam. Fire can also result if spattered oil comes in contact with open flames. Examine your Thiele tube for evidence of water droplets in the oil. If there are any, either change the oil or exchange tubes. Give the contaminated tube to your instructor. 

Because the melting point of one of the compounds is near 200 °C, do not use a liquid-filled apparatus such as a Thiele tube unless the heating medium is silicone oil. A metal block melting-point apparatus is satisfactory for determining the melting points of the semicarbazones in this experiment. 

With the Thiele tube (Fig. 39) you use hot oil to transfer heat evenly to your sample in a melting point capillary, just like the metal block of the Mel-Temp apparatus does. You heat the oil in the sidearm and it expands. The hot oil goes up the sidearm, warming your sample and thermometer as it touches them. Now, the oil is cooler and it falls to the bottom of the tube where it is heated again by a burner. This cycle goes on automatically as you do the melting point experiment in the Thiele tube. 

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