4 g. of VCl3 is treated with anhydrous HF in a nickel, sintered alumina or platinum vessel. At the start of the experiment the apparatus is flushed with dry nitrogen to displace atmospheric oxygen. During the fluorination the tube is slowly heated to 200°C. After 1.5 hours the temperature is raised to red heat. The reaction is complete when the exit gas no longer contains any HCl. The product is allowed to cool to 100°C in a stream of HF gas, after which the cooling is continued in a nitrogen stream. The yield is 95%, based on VCl3.
