Densities of molten nickel mattes
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r e s i s t a n c e type capable of o p e r a t i o n up to 1500~ with a c o n s t a n t t e m p e r a t u r e zone of about 15 cm. The f u r nace was c o n t r o l l e d to within +2~ u s i n g a t e m p e r a t u r e c o n t r o l l e r a c t i v a t e d by a P t - P t 10 pct Rh t h e r m o couple. The f u r n a c e t e m p e r a t u r e was m o n i t o r e d with a c a l i b r a t e d P t - P t 10 pct Rh t h e r m o c o u p l e . The p u r i f i e d n i t r o g e n a t m o s p h e r e was p r e p a r e d by p a s s a g e through a p y r o g a l l o l c o l u m n d r i e d over s i l i c a gel and p h o s p h o r u s pentoxide. A m e r c u r y r e s e r v o i r and e l e v a t o r w e r e a r r a n g e d for c o n t r o l of v o l u m e in the s y s t e m . The m e r c u r y e l e v a t o r was fitted with a m i c r o m e t e r a d j u s t m e n t to provide for fine p o s i t i o n i n g of the m e r c u r y and m a n o m e t e r l e v e l s . D i s t i l l e d w a t e r was used in the m a n o m e t e r . Each leg of the q u a r t z s a m p l e tube was 40 cm long with a n i n s i d e d i a m e t e r of 0.8 cm. The a v e r a g e weight of m a t t e for each e x p e r i m e n t was 30 g. The U - t u b e was
EXPERIMENTAL Materials All m a t t e s used w e r e m i x t u r e s of s y n t h e t i c Cu2S, FeS and NisS2 p r e p a r e d by h e a t i n g pure m e t a l p o w d e r s (Ni 99.79 pct p u r i t y , F e 99.88 pct p u r i t y and Cu 99.99 pct purity) with r e a g e n t grade s u l f u r in a q u a r t z tube u n d e r v a c u u m . The n i c k e l and i r o n p o w d e r s were c a r bonyl nickel powder 128 and c a r b o n y l i r o n powder MC grade supplied by the I n t e r n a t i o n a l Nickel C o m p a n y of Canada Ltd.
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Analysis The m e t a l l i c e l e m e n t s of the s y n t h e t i c s u l f i d e s and m a t t e s were d e t e r m i n e d by a t o m i c a b s o r p t i o n and the s u l f u r by a s t a n d a r d g r a v i m e t r i c method 9 T h e s e s u l f i d e s which were used for p r e p a r a t i o n of the v a r i o u s m a t t e s were n o n s t o i c h i o m e t r i c h a v i n g a n a l y s e s c o r r e sponding to the f o r m u l a s Feo.952S, CuL72S, NisS2.19 and NisS2.14 (two n i c k e l s u l f i d e s were p r e p a r e d with the f o r m e r being used in studying the Cu2S-NisS2 s y s t e m ) . Experimental Apparatus The a p p a r a t u s i l l u s t r a t e d in F i g . 1 c o n s i s t s of a f u r nace, nitrogen purification system, mercury reservoir and e l e v a t o r , m a n o m e t e r , q u a r t z U - t u b e , and t u n g s t e n probe 9 The f u r n a c e was a v e r t i c a l s i l i c o n c a r b i d e J. J. BYERLEY and N. TAKEBE are Associate Professor and Postdoctoral Fellow, respectively, Department of Chemical Engineering, University of Waterloo, Waterloo, Ontario, Canada. Manuscript submitted September 25, 1970. METALLURGICALTRANSACTIONS
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