T h e recipes given in the literaturel) for the preparation of nickel carbonyl in the laboratory are in our experience rather unsatisfactory as regards yield.Based on the observations of M a n c h o t and G a l l s ) andM i t t a s c h 3 ) from which it appears that the presence of sulphides favours the formation of nickel carbonyl from nickel and carbon monoxide, we have worked out the following recipe 4 ) .Preparation of nickel oxalafe on infusorial earth. One hundred g of infusorial earth (purified by the method of A d k i n s and C r a m e r 5 ) ) were suspended in a warm solution of 300 g of crystallise,d nickel nitrate hexahydrate, and a warm solution of 130 9 of hydrated oxalic acid was added to the boiling suspension. After filtration and washing, the precipitate was dried a t 120" until a stiff mass was obtained, 3-4 cm3 of concentrated sulphuric acid were then stirred into the mass and the drying continued until a powder was obtained.Formic acid (85 "/c) was allowed to drop from a dropping funnel into 400 cm3 of concentrated sulphuric acid in a two litre Pyrex distillation flask ( B ) .
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