Preparation of chromyl chloride
All reagents and glassware must be dry! 80 g of dry potassium dichromate and 50 g sodium chloride are well mixed and added to a 2000 ml distillation flask fitted with a dropping funnel, a condenser, and a receiver. From the dropping funnel, 150 g of fuming sulfuric acid are slowly added dropwise to the mixture of potassium dichromate and sodium chloride. Even without heated chromyl chloride starts to form which is collected in the received, which is cooled with ice-water. The reaction flask is gently heated and the reaction is continued until the content starts to foam. The obtained chromyl chloride is purified by fractional distillation, yielding dark red liquid, which fumes when exposed to the air and boils at 116° C. The chromyl chloride could be preserved in sealed tubes.
Laboratory manual of inorganic preparations, by H. T. Vulte, 150-151, 1895
Preparation of chromyl chloride is presented in the following video by Doug’s Lab.