An Improved All-glass Apparatus for the Preparation of Phosphonium Iodide

AN IMPROVED ALL-GLASS APPARATUS FOR THE PREPARATION OF PHOSPHONIUM IODIDE 

We have constructed an all-glass apparatus for the preparation of this compound (see Fig. 12). It embodies the features of Work s10 apparatus and also has some modifications which make the preparation less hazardous and less cumbersome. Higher yields were also obtained. 

The mixture10 of diphosphorus tetraiodide and white phosphorus is introduced into flask A of the apparatus, which has been previously swept with carbon dioxide. This flask is constructed so as to fit a Glas Col spherical heating mantle which enables even heating. The connections between flask A and the condenser and between the condenser and flask B are wrapped in electrical heating tape which is connected to a variable source of power. 

Hot water is slowly circulated through the condenser and returned to the hot-water bath. The glass joint connection between flask B and the condenser is heated with the heating tape to about the same temperature as the circulating 

The variable-length rubber tubing enables easy manipulation when the apparatus has to be tilted. C and D are safety traps, whereas E and F are water traps for hydrogen iodide. 

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