Preparation of Sodium Sulphide

Preparation of Sodium Sulphide. Assemble an apparatus as shown in Fig. 67. Put 0.2 g of finely triturated highly pure sulphur into test tube 1 with a ground-glass joint, and lower the tube into a beaker with a mixture of dry ice and acetone. Connect a source of dry ammonia (see Fig. 62a) to cock 

3 of the apparatus, open cock 4, and fill the apparatus with ammonia. Put 2 g of metallic sodium thoroughly purified of oxide films and washed with benzene and diethyl ether onto filter 2. Pass ammonia through the apparatus until test tube 1 is filled with liquid ammonia up to one-third of its volume, after which disconnect the apparatus for preparing ammonia. 

Close cocks 3 and 4, remove the cooling beaker from test tube 1, and put dry ice wetted with acetone into beaker 5 with double walls. 

Repeatedly remove the cooling agent and supply it to test tube 1 and beaker 5 so that the liquid ammonia will dissolve the metallic sodium on filter 2. (Open cock 4 from time to time to relieve the excess pressure of the ammonia.) 

Carefully with your instructor s assistance ) wash the vessel with small portions of ethanol because traces of unreacted metallic sodium may remain on the walls of the test tube and the filter. (When the sodium residues are slaked with ethanol, the sodium may ignite ) 

Preparation of Sulphur Chlorides, (a) Preparation of a Mixture of Sulphur Chlorides. Perform the experiment in a fume cupboard ) Melt 

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