Hydrides of Germanium, Tin, Arsenic, and Antimony

Submitted by William L. Jolly and John E. Drake Checked by Ralph RuDOLPHt and T. WartikI 

Volatile hydrides may be prepared from ether solutions by the reaction of the appropriate chlorides with lithium tetrahydroaluminate. In this general method, it is necessary to work with strictly anhydrous reagents and solvents because of the great reactivity of lithium tetrahydro-aluminate toward water. The procedures described below are believed to be much more convenient because the reducing agent employed is potassium tetrahydroborate, which is relatively insensitive toward water. Since only aqueous solutions are involved, there are no solvent-purification steps and there is no dissolution or contamination of stopcock grease, etc. 

The apparatus shown in Fig. 6 may be used for the preparation of the hydrides of germanium, tin, arsenic, 

The germane prepared has a vapor pressme of 181 mm. at —111.6° (literature, 182 mm. ). The infrared spectrum of the gas in the NaCl region shows the fundamental frequencies vz, Vi, and Vi at 2105, 943, and 815 cm. respectively. Germane is stored in a glass vessel with a greased stopcock. 

---