By Sydney Marks
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Additional info for A textbook of inorganic chemistry vol.VI part III Vanadium, Niobium, and Tantalum
Once the air has been displaced, the furnace is heated and a moderate flow of Ar and H, (50 :50) introduced at about 200”. During the subsequent heat-up, at least some of the metal will be converted to the hydride which probably enhances its reactivity. Once the temperature reaches 600-800”, the H, flow is greatly reduced and a good flow of HC1+ Ar (1 :1) is started. m Caution. The reaction is strongly exothermic, and chloride plus hydride formation may consume essentially all of the added HC1 during active periods.
Corbett, R. A. Sallach, and D. A. Lokken, Adv. Chem. , 71,56 (1967). 4. E. Warkentin and A. Simon, private communication. 5. J. D. Corbett, K. R. Poeppelmeier and R. L. Daake, Z. Anorg. , 491,51 (1982). 6. E. Warkentin and H. Anorg. , 459,187 (1979). 7. E. Warkentin and H. Biirnighausen, private communication. Trichlorides of the Rare Earth Elements, Yttrium, and Scandium 39 8. TRICHLORIDES OF THE RARE EARTH ELEMENTS, YTTRIUM,AND SCANDIUM M(s) t 3HCl(g) - MC13 t 3/2H2 Submitted by JOHN D. CORBETT.
Contamination of the contents in A during the short periods of handling in air necessary for the above steps does not seem to be a problem with well-crimped tubes except for the most susceptible systems; end-capped (B) tubes have a shorter leakage path, but these can be rapidly and directly transferred to the welder which is then evacuated to at least torr before back-filling with noble gas. Nitrogen within the tube from a dry-box atmosphere is readily removed during the evacuation and does not produce the nitride during the welding.
A textbook of inorganic chemistry vol.VI part III Vanadium, Niobium, and Tantalum by Sydney Marks