calcium turnings (99.5 purity, from same source) and red phosphorus o r resublirned arsenic o r germanium (99.999 y~L purity, from Messrs. Schuchardt) in stoichiometric proportions by heating a t l l O O 0 C for 24 h in evacuated quartz ampoules. Magnesium nitride and calcium nitride were produced by passing gaseous ammonia over magnesium or calcium turnings at 850 OC. The starting materials were mixed in I : 1 molar ratios and compressed under a pressure of 10000 kg/cmz or sintered in evacuated quartz tubes a t 1000°C for 48 h. The gases resulting from the hydrolysis were identified by mass spectroscopy [2]. In order t o preclude decomposition o f readily labile hydrides before their introduction into the spectrometer, the crystalline mixed phases were decomposed with 2 N HCI with cooling (0 "C) in an evacuated apparatus directly within the instrument. Apart from the known hydrides of phosphorus, arsenic, nitrogen, and germanium, the following products were obtained: P3HS, As3H5, and PH2AsH2 from Mg,Pz/Mg3Asz; P3H~,PH2NH2,PH(NH2)2,P(NH2)3, and PzH3NH2 from Mg3PdMg3Nz; As3H5, AsHzNH2, AsH(NHd2, and As(NH2)3 from MgsAsziMglN2; P3H5 and GeH3PHr [3] from CaGe/Ca3Pz, As3Hs and GeH3AsH2 131 from CaCe/Ca3As~; GeHlNH2 and GeH2(NH2)2 from CaGe/Ca,Nz.
Received, July 29th, 1964[Z 8211642 IEI German version: Angew. Chem. 76, 860 (1964)